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CAS No. : | 629-50-5 | MDL No. : | MFCD00008979 |
Formula : | C13H28 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IIYFAKIEWZDVMP-UHFFFAOYSA-N |
M.W : | 184.36 | Pubchem ID : | 12388 |
Synonyms : |
|
Num. heavy atoms : | 13 |
Num. arom. heavy atoms : | 0 |
Fraction Csp3 : | 1.0 |
Num. rotatable bonds : | 10 |
Num. H-bond acceptors : | 0.0 |
Num. H-bond donors : | 0.0 |
Molar Refractivity : | 64.6 |
TPSA : | 0.0 Ų |
GI absorption : | Low |
BBB permeant : | No |
P-gp substrate : | No |
CYP1A2 inhibitor : | Yes |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -2.7 cm/s |
Log Po/w (iLOGP) : | 4.03 |
Log Po/w (XLOGP3) : | 6.66 |
Log Po/w (WLOGP) : | 5.32 |
Log Po/w (MLOGP) : | 5.67 |
Log Po/w (SILICOS-IT) : | 4.88 |
Consensus Log Po/w : | 5.31 |
Lipinski : | 1.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 3.0 |
Bioavailability Score : | 0.55 |
Log S (ESOL) : | -4.52 |
Solubility : | 0.00558 mg/ml ; 0.0000303 mol/l |
Class : | Moderately soluble |
Log S (Ali) : | -6.46 |
Solubility : | 0.0000636 mg/ml ; 0.000000345 mol/l |
Class : | Poorly soluble |
Log S (SILICOS-IT) : | -5.11 |
Solubility : | 0.00144 mg/ml ; 0.00000782 mol/l |
Class : | Moderately soluble |
PAINS : | 0.0 alert |
Brenk : | 0.0 alert |
Leadlikeness : | 3.0 |
Synthetic accessibility : | 1.93 |
Signal Word: | Danger | Class: | 9 |
Precautionary Statements: | P210-P264-P280-P302+P352-P370+P378-P331-P337+P313-P305+P351+P338-P362+P364-P332+P313-P301+P310-P403+P235-P405-P501 | UN#: | 3082 |
Hazard Statements: | H227-H315-H319-H304-H410 | Packing Group: | Ⅲ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With nickel at 175 - 250℃; Hydrogenation; | ||
25.7 %Chromat. | With 60% nickel on silica; hydrogen at 232℃; Industrial scale; | The experiments were carried out in a vapor phase reactor in continuous mode (bottom-up flow). The reactor was comprised of an oil-heated 2.1 m double-walled tube with 4.11 cm inner diameter which was filled from bottom to top with 40 mL of ceramic rings (2.5-3.5 mm diameter), 0.5 L catalyst (60 wt-% Nickel on S1O2 (40 wt-%), BASF SE) and 1.8 L ceramic rings (2.5-3.5 mm diameter). After the filling the catalyst was activated by exchanging nitrogen with hydrogen and heating to 280°C (circulated oil temperature) in a stream of hydrogen of 200 Ls/h (Ls = vol ume in liters under standard conditions (p=1 atm, T=0 °C)) for 24 h. (0076) The feeds of make-up hydrogen, recycle gas and Lorol were heated to the required temperature and fed to the liquid feed evaporator The oil thermostat of the double-walled reactor tube was set to the desired reactor temperature. Via two heat exchangers the reactor output was first cooled with cooling water, then by means of a cryostat cooled to 10°C and fed into a high- pressure separator. There, separation into liquid and vapor phase was carried out. The liquid phase was depressurized into a low-pressure separator that was maintained at a temperature of 30°C and from which remaining gaseous components were vented to a flare and the liquid dis charged into a collecting vessel for crude reactor output. Via a gas compressor, the vapor phase from the high-pressure separator was recycled in a defined amount and was used as carrier gas for the feed. Via a pressure control valve excess gas was discharged into the flare for burning. Conversion and selectivity of the crude output were determined by gas chromatog raphy. (0077) Liquid feed evaporator and reactor were all set to 230°C. 300 Ls/h fresh make-up H2 (corre sponding to 600 Ls per liter of catalyst and hour) and approximately 4000 Ls/h recycle gas (cor responding to 8000 Ls per liter of catalyst and hour) and 0.3 kg/h of Lorol were fed into the reac tor. Lorol is a mixture of approx. 72 wt.-% of dodecanol and 26 wt.-% tetradecanol (containing approx. 2 wt.-% of other alcohols). The Lorol used in these experiments was obtained by hydro genation of a corresponding mixture of lauric and myristic acid being derived from palm kernel oil and coconut oil. Said palm kernel oil has been sourced from Indonesia, Malaysia, and Co lumbia. Said coconut oil has been sourced from Indonesia and the Philippines. The pressure was varied as specified in table 1. The composition of the output including conversion and se lectivity is given in table 1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With pumice stone; platinum at 220 - 230℃; Hydrogenation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With pumice stone; platinum at 220 - 230℃; Hydrogenation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
83% | With triethyl borane; tri-n-butyl-tin hydride In hexane; benzene at 20℃; for 0.333333h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | With tetraethylammonium tosylate In N,N-dimethyl-formamide electroreduction; Zn-cathode, 5.6 F/mol; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With CuBr*Me2S-LiBr; lithium thiophenoxide; magnesium 1) THF, reflux, 2 h; 2) THF, 0-18 deg C, 24 h; further reagents; Yield given. Multistep reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 27% 2: 29% | With chromium dichloride; benzaldehyde In N,N-dimethyl-formamide at 25℃; for 20h; Yield given; | |
1: 27% 2: 29% | With chromium dichloride; benzaldehyde In N,N-dimethyl-formamide at 25℃; for 20h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 29% 2: 27% | With chromium dichloride In N,N-dimethyl-formamide at 25℃; for 20h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sulfuryl dichloride In dichloromethane at 70℃; for 2.5h; UV-irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In tetrachloromethane at 0℃; Irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94% | With 2,2'-azobis(isobutyronitrile); 1,1,2,2-tetraphenyldisilane In ethyl acetate for 14h; Heating; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94% | With 2,2'-azobis(isobutyronitrile); 1,1,2,2-tetraphenyldisilane In ethyl acetate for 14h; Heating; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99% | With 2,2'-azobis(isobutyronitrile); 1,1,2,2-tetraphenyldisilane In ethyl acetate for 14h; Heating; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With nickel kieselguhr at 250 - 316℃; Hydrogenation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With air at 1130℃; Formation of xenobiotics; high pressure combustion; Further byproducts given. Title compound not separated from byproducts; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With air at 1130℃; Formation of xenobiotics; high pressure combustion; Further byproducts given. Title compound not separated from byproducts; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With air at 1130℃; Formation of xenobiotics; high pressure combustion; Further byproducts given. Title compound not separated from byproducts; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
28% | With water monomer at 250℃; for 12h; | |
With lead (IV) acetate at 120℃; for 24h; Inert atmosphere; | Thermal oxidative LTA decarboxylation of tetradecanoic acid in acid as solvent (C) The mixture of 11.42 g (50 mmol) of tetradecanoic acid and 4.43 g (10 mmol) of LTA was heated to the rate and slow stream of purified Ar was introduced for 10 min in the absence of light. Mixture was heated (120 ± 2 C) and stirred for 24 h. After completion of the reaction, to the cooled solution 50 cm3 of diethyl ether and 50 cm3 of water were added. Ether layer was removed andwashed with aqueous Na2CO3 (5%) and brine. After drying (CaSO4),the solvents were removed under reduced pressure and the productsin the residue were analyzed by analytical gas chromatography and separated by preparative gas chromatography. The results of all runs are given in Table 1. | |
With photodecarboxylase from Chlorella variabilis NC64A In dimethyl sulfoxide at 37℃; for 14h; Irradiation; Sealed tube; Enzymatic reaction; |
With Chlorella variabilis NC64A fatty acid photodecarboxylase I398L mutant at 20℃; Enzymatic reaction; | 2.6 Determination of kinetic parameters General procedure: Kinetic studies for CvFAP variants toward C7-C14 were performed in 1mL mixtures (pH 8.5) containing 900μL of enzyme and 100μL of fatty acids (1μM mutants and 4μM WT CvFAP were used, respectively, due to great differences in their catalytic activity), which incubated at 20°C for different time according to the specific substrate. The reactions were terminated by the addition of 50uL 1M NaOH, and alkane product yield was measured by GC. Kinetic parameters characterization were performed with different substrate concentrations (1-5mM). The values of Vmax and KM were calculated by the Michaelis-Menten equation. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With Dimethyldisulphide; hydrogen at 363℃; for 120h; | 1 Experiment 1; A liquid feed mixture of 69.74 wt% decalin (C10H18), 0.26wt% dimethyl disulphide (DMDS) and 30wt% tallow oil was prepared. The tallow oil comprised fatty acid chains with 12 to 20 carbon atoms (including the carboxyl carbon), the bulk of the molecules having 16 or 18 carbon atoms in the fatty acid chain (including the carboxyl carbon). The liquid mixture was fed to a reactor as illustrated in Figure 4, operating at 363°C and 30 barg (3.1 MPa) pressure, at a feed-rate of 60mL/hour. A cobalt-molybdenum on alumina catalyst was used. The liquid hourly space velocity (LHSV) of the liquid feed over the catalyst was 4 h-1. A flow of hydrogen was also fed to the reactor, such that the ratio of H2 gas volume to liquid feedstock volume was maintained at a value of 200 Nm3/m3 (gas volume at 15.6°C and 1 atm). Reaction was maintained over a period of 5 days. Liquid samples were collected daily and analysed according to a chromatographic method described in ASTM D2887, and also by GCMS. Gaseous off-gas samples were analysed using gas chromatography. The quantity of liquid product was determined gravimetrically. Off-gas volume was measured using a wet-test flow meter. The mass balance calculated from the quantities of the identified components of the obtained liquid and gaseous products was 99% with 1% standard deviation. The carbon balance was 100% with 1% standard deviation. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With Dimethyldisulphide; hydrogen;cobalt-molybdenum on alumina; at 363℃; under 75757.6 Torr; for 120h;Product distribution / selectivity; | Experiment 2; The same procedure as Experiment 1 was followed, except that the reactor pressure was maintained at 100 barg (10.1 MPa). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 26 % Chromat. 2: 10% | With buta-1,3-diene; copper dichloride In tetrahydrofuran for 6h; Heating; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
22% | With buta-1,3-diene In tetrahydrofuran at 25℃; for 3h; | |
98 % Chromat. | With 1-Phenylprop-1-yne; copper dichloride In tetrahydrofuran for 6h; Heating; | |
70 %Chromat. | With 1-Phenylprop-1-yne; copper dichloride In tetrahydrofuran for 24h; Reflux; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98 % Chromat. | With 1-Phenylprop-1-yne; copper dichloride In tetrahydrofuran for 6h; Heating; | |
35 %Chromat. | With dicarbonyl(cyclopentadienyl)iron(II) chloride; buta-1,3-diene In tetrahydrofuran at 0 - 20℃; for 24h; Inert atmosphere; Schlenk technique; | Typical procedure for the iron-catalyzed cross-coupling General procedure: To a flame-dried Schlenk tube containing CpFe(CO)2Cl (6) (10.3 mg, 0.05 mmol),3-bromopropyl phenyl ether (1j) (223 mg, 1.04 mmol), THF (0.25 mL), n-BuMgCl (2a)(2M in THF, 0.75 mL, 1.5 mmol), and 1,3-butadiene (90 mL as gas, 4.0 mmol) wereadded successively at -78 C followed by stirring at 0 °C for 2 h and rt for 22 h. Thereaction was quenched by the addition of sat NH4Cl aq., extracted with Et2O (10 mL x3), concentrated, and purified by PTLC (eluent: hexane/Et2O = 99/1) to obtain heptylphenyl etherS2 (3ja) as yellow oil (79.5 mg, 40%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98 % Chromat. | With 1-Phenylprop-1-yne; copper dichloride In tetrahydrofuran for 6h; Heating; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | With buta-1,3-diene; nickel dibromide In tetrahydrofuran at 0℃; for 0.25h; | |
99 % Chromat. | With 1-Phenylprop-1-yne; copper dichloride In tetrahydrofuran at 25℃; for 0.25h; | |
91 %Chromat. | With LaFe0.80Ni0.20O3; buta-1,3-diene at 20℃; for 5h; | General procedures for Ni-perovskite catalyzed cross-coupling reactions. General procedure: A 20 mL tube was charged with the alkyl halides (1 mmol) and alkyl Grignard reagent (1.3 mmol) and cooled to -78 °C, and then 1,3-butadiene (50 mol %) was added. After addition of LaFe0.8Ni0.2O3 (LFNO) (10 mg, 0.8 mol %, 0.46 mg Ni), the mixture was stirred at rt for 5 h. It was quenched with water (1 mL) at the same temperature and then diluted with diethyl ether (5 mL), and the supernatant liquid was passed through a 0.45 μm syringe filter and washed with diethyl ether (10 mL). The mixture was washed with 1 N HCl (2 mL) followed by water (5 mL) and the aqueous layer was back extracted with diethyl ether (10 mL). The combined organic layers were dried (MgSO4) and evaporated to give the crude product, which was analyzed by GC using octane as an internal standard. |
40 %Chromat. | With 1-Phenylprop-1-yne; copper dichloride In tetrahydrofuran at 40℃; for 48h; | |
54 %Chromat. | With dicarbonyl(cyclopentadienyl)iron(II) chloride; buta-1,3-diene In tetrahydrofuran at 0 - 20℃; for 24h; Inert atmosphere; Schlenk technique; | Typical procedure for the iron-catalyzed cross-coupling General procedure: To a flame-dried Schlenk tube containing CpFe(CO)2Cl (6) (10.3 mg, 0.05 mmol),3-bromopropyl phenyl ether (1j) (223 mg, 1.04 mmol), THF (0.25 mL), n-BuMgCl (2a)(2M in THF, 0.75 mL, 1.5 mmol), and 1,3-butadiene (90 mL as gas, 4.0 mmol) wereadded successively at -78 C followed by stirring at 0 °C for 2 h and rt for 22 h. Thereaction was quenched by the addition of sat NH4Cl aq., extracted with Et2O (10 mL x3), concentrated, and purified by PTLC (eluent: hexane/Et2O = 99/1) to obtain heptylphenyl etherS2 (3ja) as yellow oil (79.5 mg, 40%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 2: 83 percent / n-Bu3SnH, Et3B / benzene; hexane / 0.33 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
EXAMPLE II Synthesis of 4,4'-Bis-[9-(3,6-diphenylcarbazolyl)]-1-1,1'-biphenyl In a 50 milliliter round bottom flask there were added 4,4'-diiodo-1,1'-biphenyl (2.1 grams), 3,6-diphenyl carbazole (3.3 grams), potassium carbonate powder (1.4 grams), copper sulfate pentahydrate (0.06 grams), and 5 milliliters of tridecane. The resulting mixture was heated to 230° C. and stirred at this temperature under argon for 24 hours. After cooling to room temperature (~23° C.), the solids content resulting was ground into slurry, which slurry was then transferred to a filtration funnel, washed with hexane to remove the tridecane, followed by washing with 3 percent hydrochloric acid and water. The solid resulting was then dissolved in hot toluene. The insoluble residue was filtered hot. After cooling to room temperature, the product was crystallized from the solution to yield 2.3 grams of 4,4'-bis-[9-(3,6-diphenylcarbazolyl)]-1,1'-biphenyl as a yellowish powder. This compound had a melting point of 294° C. Its chemical structure was confirmed by proton analysis. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With carbon dioxide; 1,8-diazabicyclo[5.4.0]undec-7-ene In tetrahydrofuran | 2 EXAMPLE 2 EXAMPLE 2 N-benzyl-N-ethyl allyl carbamate: Into a Fischer-Porter bottle Was added 13.5 g (0.1 mol) N-benzyl-N-ethyl amine, 16 1 g (0.106 mol) DBU and 1 g (5.38 mmol) tridecane (as G.C. internal standard). To this was added 65 mL anhydrous THF giving a clear solution. The Fischer-Porter bottle was attached to a pressure head and ca. 35 psig carbon dioxide was added above the solution at room temperature with stirring. Upon addition of carbon dioxide, the solution warmed slightly and after 2 hours absorption of CO2 had ceased. Into a second Fischer-Porter bottle was added 100 mg (0.11 mmol) of Pd2 dba3 and 108 mg (0.27 mmol) of DIPHOS (bis-diphenylphosphinoethane). This Fischer-Porter bottle was attached to a pressure head and the apparatus was flushed with carbon dioxide. Anhydrous THF (45 mL) was added to this mixture giving a purple solution which slowly turned yellow. After 15 minutes 16.35 g (0.214 mol) allyl chloride was added and the reaction mixture was allowed to stir at room temperature for 15 minutes. The carbamate salt solution was added to the palladium-DIPHOS-allyl chloride mixture at room temperature with rapid stirring using excess carbon dioxide pressure to force the carbamate solution into the reactor with the catalyst. A head pressure of 80 psig carbon dioxide was then added above the reaction mixture and the reaction was allowed to stir at room temperature for 21 hours during which time a white solid precipitated. After this time, the pressure was released and the yellow solution was filtered through silica gel (this inactivates the catalyst). The filtrate was concentrated leaving a yellow oil. Distillation at 5 torr (125°-13020 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | With trichlorophosphate In carbamic acid cyclohexyl ester; acetonitrile | 3 EXAMPLE 3 EXAMPLE 3 This example demonstrates the production of cyclohexyl isocyanate from cyclohexylamine using P1 -tBu as the base and phosphorus oxychloride as the "dehydrating agent". A Fischer-Porter bottle was charged with 0.15 g (1.5 mmol) of cyclohexyl amine, 0.99 g of P1 -tBu (3 mmol), 10 mL of acetonitrile and 71 mg (0.5 mmol) of tridecane as an internal standard. The bottle was pressurized to 80 psig with carbon dioxide and the solution was stirred for 30 minutes at room temperature. A second Fischer-Porter bottle was charged with 0.14 mL (1.5 mmol) of phosphorus oxychloride and 10 mL of acetonitrile then pressurized to 80 psig with CO2. The two solutions were cooled to 0° C. in an ice bath for 10 minutes after which time the cyclohexyl carbamate solution was added rapidly to the POCl3 solution. An aliquot was taken after five minutes and diluted with diethyl ether prior to G.C. analysis which indicated a yield of 98% cyclohexyl isocyanate. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
11% | In n-octyl carbamate; acetonitrile | 6 EXAMPLE 6 EXAMPLE 6 This example demonstrates the production of octyl isocyanate from octyl amine using P1 -tBu as the base and SO3 -NMe3 as the "dehydrating agent". A Fischer-Porter bottle was charged with 0.55 g (4.2 mmol) of octyl amine, 0.99 g of P1 tBu (3 mmol), 25 mL of acetonitrile and 130 mg (0.84 mmol) of tridecane as an internal standard. The bottle was pressurized to 80 psig with carbon dioxide and the solution was stirred for 30 min. at room temperature. A second Ficher-Porter bottle was charged with 0.65 g (4.7 mmol) of sulfur trioxide trimethylamine adduct (SO3 -NMe3) and 20 mL of acetonitrile then pressurized to 80 psig with CO2. The two solutions were cooled to 0° C. in an ice bath for 10 min after which time the octyl carbamate solution was added rapidly to the SO3 -NMe3 suspension. An aliquot was taken after five minutes and diluted with diethyl ether prior to G.C. analysis which indicated a yield of 11% octyl isocyanate. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
15% | With triethylamine In water; acetonitrile | 5 EXAMPLE 5 EXAMPLE 5 This example demonstrates the production of octyl isocyanate from octyl amine using P1 -tBu as the base and P2 O5 as the "dehydrating agent". A Fischer-Porter bottle was charged with 0.65 g (5 mmol) of octyl amine, 1.17 g of P1 -tBu (5 mmol), 0.51 g of triethylamine, 25 mL of acetonitrile and 184 mg (1 mmol) of tridecane as an internal standard. The bottle was pressurized to 80 psig with carbon dioxide and the solution was stirred for 30 minutes at room temperature. A second Fischer-Porter bottle was charged with 4 g (28 mmol) of P2 O5 (phosphorus pentoxide), 0.86 mL water, 4 mL of triethylamine and 25 mL of acetonitrile then pressurized to 80 psig with CO2. The P2 O5 /water/triethylamine mixture gave a dark brown solution and the carbamate solution was added rapidly to this mixture at room temperature. An aliquot was taken after five minutes and diluted with diethyl ether prior to G.C. analysis which indicated a yield of 15% octyl isocyanate. The reaction mixture was stirred for an additional 18 hours during which time the yield of octyl isocyanate increased to 98.8% by G.C. analysis. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate In 3,4-dimethyl-N-(p-tolyl)aniline | 1.3 (3) (3) Synthesis of 3,4,4',4"-tetramethylphenylamine (CT-3) In a one-liter three-neck flask were placed 50 g of 3,4,4'-trimethyldiphenylamine, 62 g of p-iodotoluene, 33 g of anhydrous potassium carbonate, 2 g of copper sulfate petahydrate and 10 ml of n-tridecane, and after carrying out the reaction for 120 hours at 200° C. under a nitrogen gas stream, the reaction mixture was cooled to room temperature. The reaction mixtue was subjected to a column purification using a mixed solvent of n-hexane and toluene (volume ratio: 10/1) with activated alumina and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of ethyl acetate and ethanol to provide 52 g of 3,4,4',4"-tetramethyltriphenylamine. (Melting point 107° to 109° C., colorless crystals, IR spectrum shown in FIG. 1.) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate In bis-(3,4-dimethyl-phenyl)-amine | 3.1 EXAMPLE 3 In one-liter three-neck flask were placed 50 g of 3,3',4,4'-tetramethyldiphenylamine, 58 g of p-iodotoluene, 30 g of anhydrous potassium carbonate, 2 g of copper sulfate pentahydrate and 10 ml of n-tridecane, and after carrying out the reaction for 40 hours at 200° C. under a nitrogen gas stream, the reaction mixture was cooled to room temperature. The reaction mixture was subjected to a column purification (solvent: n-hexane/toluene=10/1) with activated alumina and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of ethyl acetate and ethanol to provide 58 g of 3,3',4,4',4"-pentamethyltriphenylamine. (Melting point 115° to 117.5° C., colorless crystals, IR spectrum shown in FIG. 3.) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 1-methyl-pyrrolidin-2-one; nitrogen; p-benzoquinone; lithium chloride; sodium chloride | 6 EXAMPLE 6 EXAMPLE 6 To a solution of N-methylpyrrolidone (0.75 ml) and Li2 MoO4 (0.11 gm) was added PdSO4 (0.024 gm), LiCl (0.0054 gm), benzoquinone (0.03 gm) and H2 O (0.075 ml). The solution was gently but continuously stirred for about 5 minutes using nitrogen as an inert purging gas. Myrcene (0.066 ml) was added and the solution was heated to about 90° C., for about 2.5 hrs, with gentle and continuous stirring. Tridecane (0.013 gm) was then added to the mixture as an internal standard, and the solution was transferred to a separation funnel, rinsed with toluene (1.5 ml) and extracted five times using a NaCl/H2 O solution. The organic phase was then dried over K2 CO3, and the resulting product analyzed substantially as described in Example 1. The resulting yield of citral was 34%, with a selectivity of 17%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 1-methyl-pyrrolidin-2-one; sodium chloride In water; toluene | 1 EXAMPLE 1 EXAMPLE 1 To a solution of N-methylpyrrolidone (0.75 ml) and Li2 MoO4 (0.11 gm) was added PdCl2 (CH3 CN)2 (0.03 gm) and water (0.075 ml). The solution was gently but continuously stirred using a magnetic stirrer for about 5 minutes while nitrogen was employed as an inert purging gas. Myrcene (0.066 ml) was then added to the solution and the mixture was heated to about 90° C. for about 2.5 hrs, with gentle and continuous stirring. Tridecane (0.014 gm) was then added to the mixture as an internal standard, and the solution was transferred to a separation funnel. Toluene (1.5 ml) was added, and the solution was extracted five times using a NaCl/H2 O mixture. The organic phase was then dried over K2 CO3. The resulting yield of citral was 44%, with a selectivity of 26%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium hydroxide; dimethyl sulfoxide In chloroform | 10 Preparation of 2-methoxy-6-(methylthiomethyl)aniline Using n-Butanesulfonic Acid in Chloroform EXAMPLE 10 Preparation of 2-methoxy-6-(methylthiomethyl)aniline Using n-Butanesulfonic Acid in Chloroform To a solution of 1.429 g (0.018 moles) of dry dimethyl sulfoxide and 2.27 g (0.015 moles) of dry n-butanesulfonic acid in 13 ml of dry chloroform, was added 2.2110 g (0.0148 moles) of o-methoxyphenyl isocyanate. After thirty minutes at room temperature, the reaction mixture was refluxed for three and a half hours. After cooling to room temperature, the reaction mixture was poured into 180 ml of ice-cold 10% aqueous sodium hydroxide solution. After extracting with methylene chloride, the organic layer was dried over anhydrous sodium carbonate, filtered and 0.10 g of succinimide was added. The resulting solution was concentrated to 100 ml and then refluxed for twenty hours. This solution was cooled, extracted with 10% aqueous sodium hydroxide solution and the organic layer dried over anhydrous magnesium sulfate and filtered. At this point, tridecane was added as an internal standard and the solution was analyzed by gas chromatography. In this manner, there was obtained 0.338 g (22.4%) of o-methoxyaniline and 1.8319 g (67.6%) of 2 -methoxy-6-(methylthiomethyl)aniline. The results are included in Table II. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
36% | With 1-methyl-pyrrolidin-2-one; sodium hydrogencarbonate; N-ethyl-N,N-diisopropylamine; triphenylphosphine | 121 EXAMPLE 121 EXAMPLE 121 0.1 g Palladium acetate, 0.36 g triphenylphosphine, 7.9 g bromobenzene, 0.2 g diisopropylethylamine, 4.4 g sodium bicarbonate and 20 ml N-methylpyrrolidinone were heated to 140° with stirring under nitrogen together with 2 grams of tridecane as internal standard. 4.4 g Allyl alcohol was added gradually at temperature over a period of 25 minutes to give a 13% yield of hydratropic aldehyde and a 36% yield of phenyl propionaldehyde based on bromobenzene. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate; In water; toluene; | Preparation of 5,11-di-m-tolyl-<strong>[6336-32-9]5,11-dihydro<strong>[6336-32-9]indolo[3,2-b]carbazole</strong></strong>: A 200-milliliter 3-necked round bottom flask equipped with a mechanical stirrer, reflux condenser, and argon inlet was purged with argon and then charged with <strong>[6336-32-9]5,11-dihydro<strong>[6336-32-9]indolo[3,2-b]carbazole</strong></strong> (5.1 grams, 0.02 mol), 3-iodotoluene (8.69 grams, 0.04 mol), copper sulfate pentahydrate (0.25 gram, 1.0 mmol), potassium carbonate (5.52 grams, 0.04 mol), and n-tridecane (5.0 milliliters). Under an argon atmosphere, the reaction mixture was heated to about 250°C with a heating mantle and allowed to proceed at this temperature to completion in about 6 hours. The mixture was cooled to about 100°C, and 100 milliliters of toluene and 15 milliliters of water were then added with vigorous stirring. The resulting two phase mixture was transferred into a separatory funnel and the layers separated. The organic phase, which contained the desired product, was washed with water, and treated with 25 grams of alumina under an argon atmosphere, and filtered. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate; In water; toluene; | EXAMPLE III Synthesis of 5,11-di-1-naphthyl-<strong>[6336-32-9]5,11-dihydro<strong>[6336-32-9]indolo[3,2-b]carbazole</strong></strong> (3): A 200 milliliter 3-necked round bottom flask equipped with a mechanical stirrer, reflux condenser, and argon inlet was purged with argon and then charged with <strong>[6336-32-9]5,11-dihydro<strong>[6336-32-9]indolo[3,2-b]carbazole</strong></strong> (5.1 grams, 0.02 mol), 1-iodonaphthalene (10.16 grams, 0.04 mol), copper sulfate pentahydrate (0.25 gram, 1.0 mmol), potassium carbonate (5.52 grams, 0.04 mol), and n-tridecane (5.0 milliliters). Under an argon atmosphere, the reaction mixture was heated to about 250°C with a heating mantle and allowed to proceed at this temperature to completion in about 6 hours. The reaction mixture was cooled to about 100°C, and 100 milliliters of toluene and 15 milliliters of water were then added with vigorous stirring for 30 minutes. The resulting two phase mixture was transferred into a separatory funnel and the layers separated. The organic phase which contains the desired product was washed with water, treated with 25 grams of alumina under an argon atmosphere, and filtered. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 89% 2: 2.1% | With hydrogen at 240℃; for 12h; | 1 1000 grams of 1-tetradecanol (4.7 mol; Lorol C 14 from Cognis) were introduced into a stirrable pressure vessel with 10 grams of a nickel catalyst (Ni-5249 P from Engelhard; Ni content=63% by weight) and heated to 240° C. Hydrogen was then added over a period of 12 hours under a pressure of 20 bar through a gas dispersion tube and, at the same time, the reaction gases were removed through a valve in the lid of the reactor. The product was then cooled, drained off and filtered. A yield of 845 grams of reaction product was obtained.GC analysis revealed the following composition: 89.0% tridecane, 2.1% tetradecane, 4.1% 1-tetradecanol, 4.2% dimeric reaction products.The reaction product was then fractionated by distillation to pure tridecane and deodorized with nitrogen. A colorless, thinly liquid and substantially odorless product was obtained. |
With hydrogen In n-heptane at 199.84℃; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen at 300℃; for 5h; | 7 Examples 5 through 8Examples 5 through 8 illustrate hydrocracking and hydroisomerization in a single step. Results from Examples 5 through 8 are summarized in Table 1 below. The Examples used a feed comprised of a mixture of hydrocarbons: 3% n-C19, 91% n-C18, and 6% n-C17) prepared by hydrodeoxygenating canola oil in a continuous flow reactor using a commercial nickel/molybdenum on alumina catalyst at a temperature 325° C. and pressure 1500-2000 psig (10,400-13,900 kPa), followed by distilling the product to obtain a predominantly n-C18 cut.This feed mixture (100 g) was reacted with reduced Ni/NiO/MgO/SiO2/graphite catalyst (Pricat Ni 55/5 P catalyst) (2.5 g) individually mixed with 4 different zeolite powders (2.5 g), specified in Table 1. These Examples were conducted at 300° C. and 1500 to 2000 psig (13,900 kPa) under hydrogen in 400-cc pressure tubes for 5 hours under constant shaking. H2 uptake was less than those in Examples 1 through 4. As can be seen from table 1, linear hydrocarbons similar to those produced in Examples 1 through 3, undergo hydroisomerization and hydrocracking using catalysts comprising nickel supported on alumina combined with a zeolite. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen at 325℃; for 5h; | 19 Example 19The process of Example 18 was repeated using the same equipment, pressure, and temperature except the catalyst was Grace-Davidson AT 535 catalyst (5 g) and crude soybean oil from Perdue Farms (50 g) was used. The catalyst was sulfided, as described hereinabove. The reaction products were analyzed by GC-FID to obtain the following linear paraffin distribution by weight: C18+=2.0%, C18=78.0%, C17=8%, C16=10%, C15=1.1%, C14=0.2%, C13=0.2%, C12=0.1%, C11=0.1%, C7-10=0.3%. The C18:C17 ratio is approximately 9.75, and C16:C15 ratio is greater than 9. | |
With hydrogen at 325℃; for 5h; | 20 Example 20The process of Example 19 was repeated using the same equipment, pressure, and temperature except Grace-Davidson AT 792 catalyst (5 g,) was used. The catalyst was sulfided, as described hereinabove. The reaction products were analyzed by GC-FID to obtain the following linear paraffin distribution by weight: C18+=1.8%, C18=82.4%, C17=3.3%, C16=11.2%, C15=0.5%, C14=0.2%, C13=0.1%, C12=0.1%, C11=0.1%, C7-10=0.3%. The C18:C17 ratio is approximately 25, and C16:C15 ratio is greater than 22. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen at 325℃; for 5h; | 18 Example 18The process of Example 13 was repeated using the same equipment, pressure, temperature, and catalyst (5 g), except a 50:50 chicken fat to soybean oil mixture (50 g, mixed in-house with chicken fat and soybean oil obtained from Perdue Farms of Salisbury, Md.) was used. The reaction products were analyzed by GC-FID to obtain the following linear paraffin (hydrocarbon) distribution by weight: C18+=2.1%, C18=69.6%, C17=7.2%, C16=18.5%, C15=1.9%, C14=0.5%, C13=0.1% C12=0.1%. The C18:C17 ratio is approximately 9.7, and C16:C15 ratio is greater than 2.5. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen at 325℃; for 5h; | 14 Example 14The process of Example 13 was repeated using the same equipment, pressure, temperature, and catalyst (5 g), except refined coconut oil, (50 g, obtained from Spectrum Chemicals of Gardena, Calif.) was used. The reaction products were analyzed by GC-FID to obtain the following linear paraffin (hydrocarbon) distribution by weight: C18=9%, C17=1%, C16=9%, C15=1%, C14=17.5, C13=2, C12=43.5%, C11=4, C10=5.5, C9=0.5, C8=6.5%, C7=0.5%. The C18:C17 ratio is approximately 9, C16:C15 ratio is 9, C14:C13 ratio is approximately 9, C12:C11 ratio is approximately 11, C10:C9 ratio is 11, and C8:C7 ratio is 13. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96% | With N,N,N,N,-tetramethylethylenediamine; cobalt(II) chloride; lithium iodide In tetrahydrofuran at 10℃; for 1h; Inert atmosphere; chemoselective reaction; | |
55.8% | With 2,3-dimethyl-2,3-diaminobutane; [ICo(N-bis(diisopropylphosphino)-3,5-dimethylaniline(-H))2(μ-I)(η2-N-bis(diisopropylphosphino)-3,5-dimethylaniline(-H))] In tetrahydrofuran | |
99.1 %Chromat. | With N,N,N,N,-tetramethylethylenediamine; ZrCl(N(iPr)P(iPr)2)CoI In tetrahydrofuran at 20℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97% | With N,N,N,N,-tetramethylethylenediamine; cobalt(II) chloride; lithium iodide In tetrahydrofuran at 10℃; for 1h; Inert atmosphere; chemoselective reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With phosphorus pentachloride; trichlorophosphate In isopropyl alcohol | 3 Synthesis of Compound 3 A mixture of N-(3,5-dicyclohexyl-4-yl)benzamide (2.1 g, 4.8 mmol), phosphorus oxychloride (10 mL) and phosphorus pentachloride (1.0 g, 4.8 mmol) was stirred at reflux for 4 h. The phosphorous oxychloride was removed in vacuo. To the crude brown solid was added 25 mL of isopropanol and aminoacetaldehyde dimethyl acetal (10.4 mL, 96.0 mmol). This was stirred at ambient temperature for 22 h. The mixture was concentrated on the rotary evaporator. To the residue was added a mixture of 30 mL of isopropanol and 30 mL of con HCl. This was stirred at 90° C. for 22 h. The mix was then cooled to ambient temperature and the pH was adjusted to 10 using 1N NaOH. The product was extracted with dichloromethane and purified on a silica gel column. Elution with dichloromethane and ethyl acetate (95:5) yielded 1.4 grams (64%) of the product. 1H NMR confirmed the structure. Synthesis of Compound 3. Into a Schlenk tube were added a stir bar, 1-(3,5-dicyclohexylbiphenyl-4-yl)-2-phenyl-1H-imidazole (3.1 grams, 6.7 mmol), iridium (III) acetylacetonate (0.66 grams, 1.3 mmol) and tridecane (0.3 mL). This was evacuated and backfilled with nitrogen. The reaction was stirred at 250° C. for 48 h. The product was purified using column chromatography. Elution with hexanes and dichloromethane (1:1) gave 1.88 grams (92%) of the product as a yellow solid. 1H NMR confirmed structure. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium permanganate In nitrogen; ethyl acetate; acetonitrile | 3 Synthesis of Compound 3 1-(2,4-diisopropyldibenzo[b,d]furan-1-yl)-2-phenyl-4,5-dihydro-1H-imidazole (4.7 g, 12 mmol) was dissolved in 100 mL acetonitrile. To the stirred solution fine mixture of KMnO4 (3.8 g, 24 mmol) and 4 g montmorillonite K10 clay was added in small portions and the reaction mixture was stirred for 2 h. At the end, reaction was quenched with MeOH and filtered thru a Celite pad. Crude product was purified by flash chromatography over silica gel with 80% DCM/Hexane to 80% DCM/ethylacetate. 3 g light yellow color oil was isolated. This oil was further purified by reverse phase chromatography. Target compound (1.3 g, 28% yield) was isolated as white solid. Synthesis of Compound 3. 1-(2,4-diisopropyldibenzo[b,d]furan-1-yl)-2-phenyl-1H-imidazole (1.2 g, 3 mmol), Ir(acac)3 and 100 μL tridecane were added in a Schlenk flask and purged with nitrogen. Reaction mixture was heated to 250° C. for 40 h. Cooled reaction mixture was chromatographed over silica gel with 1:1 DCM/hexanes. After sublimation, target compound (0.12 g, 14% yield) was obtained as yellow color crystal. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | 5 Synthesis of Compound 5 Synthesis of Compound 5. (1-(2,4-diisobutyldibenzo[b,d]furan-3-yl)-2-phenyl-1H-imidazole 1.97 g, 4.67 mmol), tridecane (0.1 mL), and Ir(acac)3 (0.44 g, 0.899 mmol) were added to a Schlenk tube. The tube was evacuated and refilled with nitrogen. The process was repeated three times. The reaction was heated up to 250° C. for 40 h. After cooled to room temperature, the reaction was diluted with dichloromethane and purified by silica gel column chromatography using 1:1 hexanes and dichloromethane as eluent. 0.7 g (54% yield) of product was obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium permanganate In methanol; dichloromethane; acetonitrile | 2 Synthesis of Compound 2 1-(1,3-diisopropyldibenzo[b,d]furan-2-yl)-2-phenyl-4,5-dihydro-1H-imidazole (4.78 g, 12.05 mmol) in 70 mL of acetonitrile and 70 mL of dichloromethane were added to a 1 L round bottom flask. Potassium permanganate (3.81 g, 24.11 mmol) was ground in a mortar and pestle. Monmorilonite K was added and was ground together finely with the potassium permanganate. This mixture was added to the solution in portions over 0.5 hours. Reaction was done 1 h after first addition. 100 mL of methanol was added and stirred for 1 h. The solid was filtered through Celite. The material was purified using a 200 g Varian column eluting with 20% ethyl acetate/hexanes. 2.1 g (44% yield) of product was obtained after column. Synthesis of Compound 2. 1-(1,3-diisopropyldibenzo[b,d]furan-2-yl)-2-phenyl-1H-imidazole (2.1 g, 5.32 mmol) and tris(acetylacetonate)iridium (III) (0.521 g, 1.065 mmol) were added to a Schlenk tube. 1 mL of tridecane was added. The reaction flask was evacuated and backfilled with nitrogen. The process was repeated 3 times. The reaction was heated up to 255 degrees under nitrogen for 70 h. After completion, the reaction mixture was diluted with dichloromethane and coated on Celite. The product was columned with 2:3 dichloromethane and hexanes. 1.0 g (68% yield) of product was obtained after column. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | With di-tert-butyl peroxide; tributylmethylammonium hypophosphite at 100℃; for 1h; | Typical procedure for deoxygenation of alcohols with TBMAP: a mixture of 1,2:5,6-di-O-isopropylidene3-O-(methylthio)thiocarbonyl-α-d-glucofuranose (6a) (547 mg, 1.56 mmol), TBMAP (2.07 g, 7.81 mmol) and (tBuO)2 (71 μL, 0.39 mmol) was heated at 100 °C for 1 h. After completion of reaction, mixture was diluted with CH2Cl2, then washed with aqueous Na2S2O3 solution, dried over MgSO4, and evaporated the solvent in vacuo. The residue was purified by flash column chromatography over silica gel (n-hexane/EtOAc, 7:3) to furnish 3-deoxy-1,2:5,6-di-O-isopropylidene-α-d-glucofuranose (7a) (309 mg, 81%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 59% 2: 23.6% 3: 14.3% | With C31H37ClN3NiO2(1-)*Li(1+) In tetrahydrofuran at 25℃; for 0.333333h; Inert atmosphere; Overall yield = 97.5 %; | 2.4 Cross coupling of CH2Cl2 with butylmagnesium chloride General procedure: Cross-coupling reactions of Grignard reagents with CH2Cl2 were performed according to the following general method. Catalyst 2 (1.0 mg, 1.74 μmol) in 1.0 mL THF was added using a gas-tight syringe to a 5 mL round bottom flask purged with N2. To this solution, 2 M n-butylmagnesium chloride in THF (0.42 mL, 0.84 mmol) was added. CH2Cl2 (27 μL, 0.42 mmol) in 2 mL THF was added to the reaction mixture. Samples were collected for analysis after 20 min. At the end of the reaction, excess Grignard reagent was destroyed using methanol and the reaction products were analyzed by GC-MS using an internal standard to quantify product formation. |
With C31H37ClFeN3O2 In tetrahydrofuran at 25℃; for 0.0833333h; Inert atmosphere; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 9.3% 2: 65.2% 3: 21.4% | With C31H37ClN3NiO2(1-)*Li(1+) In tetrahydrofuran at 25℃; for 0.333333h; Inert atmosphere; | 2.5 Cross coupling of CHCl3 and CCl4 with Grignard reagent General procedure: Cross-coupling reactions of Grignard reagents with CHCl3 and CCl4 were performed according to the following general method. Catalyst 2 (1 mg, 1.74 μmol) in 1 mL THF was added using a gas-tight syringe to a 5 mL round bottom flask purged with N2. To this solution 2 M n-butylmagnesium chloride in THF (0.63 mL, 1.26 mmol) was added. CHCl3 (34 μL, 0.42 mmol) was added to the reaction mixture. In the case of reactions with CCl4 (40 μL, 0.42 mmol), 1.68 mmol of Grignard reagent was added. Samples were collected for analysis after 20 min. At the end of the reaction, excess Grignard reagent was destroyed using methanol and the reaction products were analyzed by GC-MS using an internal standard to quantify product formation. |
With C31H37ClFeN3O2 In tetrahydrofuran at 25℃; for 0.0833333h; Inert atmosphere; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 78.6% 2: 13.1% 3: 5.8% | With C31H37ClN3NiO2(1-)*Li(1+) In tetrahydrofuran at 25℃; for 0.333333h; Inert atmosphere; Overall yield = 99.9 %; | 2.5 Cross coupling of CHCl3 and CCl4 with Grignard reagent General procedure: Cross-coupling reactions of Grignard reagents with CHCl3 and CCl4 were performed according to the following general method. Catalyst 2 (1 mg, 1.74 μmol) in 1 mL THF was added using a gas-tight syringe to a 5 mL round bottom flask purged with N2. To this solution 2 M n-butylmagnesium chloride in THF (0.63 mL, 1.26 mmol) was added. CHCl3 (34 μL, 0.42 mmol) was added to the reaction mixture. In the case of reactions with CCl4 (40 μL, 0.42 mmol), 1.68 mmol of Grignard reagent was added. Samples were collected for analysis after 20 min. At the end of the reaction, excess Grignard reagent was destroyed using methanol and the reaction products were analyzed by GC-MS using an internal standard to quantify product formation. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With C31H37ClFeN3O2 In tetrahydrofuran at 25℃; for 0.0833333h; Inert atmosphere; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With Mg-Zr oxide supported on high surface-area grahite100 In water at 49.84℃; for 24h; Inert atmosphere; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 83 %Chromat. 2: 6.7 %Chromat. | With acetylacetonatodicarbonylrhodium(l); 1-hydroxytetraphenylcyclopentadienyl(tetraphenyl-2,4-cyclopentadien-1-one)-μ-hydrotetracarbonyldiruthenium(II); carbon monoxide; C70H72O2P2; hydrogen In 1,4-dioxane at 120℃; for 36h; Inert atmosphere; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen at 325℃; Autoclave; | General procedure: Oleic acid (90%, Alfa-Aesar) was used as the unsaturated fattyacid. Pt/SAPO-11 was pre-activated in the oven for 3 h at 150C.The decarboxylation reactions were conducted in a 250 ml stainlesssteel, high pressure autoclave batch reactor (Parr model 4576A).Oleic acid and Pt/SAPO-11 were loaded into the reactor with a massratio of 18:1. Before the reaction started, the air in the reactor wasremoved by flushing with CO2or H2. The pressure was increased tothe desired reaction pressure (usually 20 bar). Under constant stir-ring conditions, the reactor was heated at a rate of 10C/min to thereaction temperature (200-325C) and this temperature was keptconstant during the reaction. Reaction of oleic acid with Pt-aluminawas carried out in a similar manner. After the reaction, the catalystparticles were separated, by filtration, from the liquid product andwashed with acetone for further characterizatio |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen at 325℃; Autoclave; | General procedure: Oleic acid (90%, Alfa-Aesar) was used as the unsaturated fattyacid. Pt/SAPO-11 was pre-activated in the oven for 3 h at 150C.The decarboxylation reactions were conducted in a 250 ml stainlesssteel, high pressure autoclave batch reactor (Parr model 4576A).Oleic acid and Pt/SAPO-11 were loaded into the reactor with a massratio of 18:1. Before the reaction started, the air in the reactor wasremoved by flushing with CO2or H2. The pressure was increased tothe desired reaction pressure (usually 20 bar). Under constant stir-ring conditions, the reactor was heated at a rate of 10C/min to thereaction temperature (200-325C) and this temperature was keptconstant during the reaction. Reaction of oleic acid with Pt-aluminawas carried out in a similar manner. After the reaction, the catalystparticles were separated, by filtration, from the liquid product andwashed with acetone for further characterizatio |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen at 325℃; Autoclave; | General procedure: Oleic acid (90%, Alfa-Aesar) was used as the unsaturated fattyacid. Pt/SAPO-11 was pre-activated in the oven for 3 h at 150C.The decarboxylation reactions were conducted in a 250 ml stainlesssteel, high pressure autoclave batch reactor (Parr model 4576A).Oleic acid and Pt/SAPO-11 were loaded into the reactor with a massratio of 18:1. Before the reaction started, the air in the reactor wasremoved by flushing with CO2or H2. The pressure was increased tothe desired reaction pressure (usually 20 bar). Under constant stir-ring conditions, the reactor was heated at a rate of 10C/min to thereaction temperature (200-325C) and this temperature was keptconstant during the reaction. Reaction of oleic acid with Pt-aluminawas carried out in a similar manner. After the reaction, the catalystparticles were separated, by filtration, from the liquid product andwashed with acetone for further characterizatio |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen at 325℃; Autoclave; | General procedure: Oleic acid (90%, Alfa-Aesar) was used as the unsaturated fattyacid. Pt/SAPO-11 was pre-activated in the oven for 3 h at 150C.The decarboxylation reactions were conducted in a 250 ml stainlesssteel, high pressure autoclave batch reactor (Parr model 4576A).Oleic acid and Pt/SAPO-11 were loaded into the reactor with a massratio of 18:1. Before the reaction started, the air in the reactor wasremoved by flushing with CO2or H2. The pressure was increased tothe desired reaction pressure (usually 20 bar). Under constant stir-ring conditions, the reactor was heated at a rate of 10C/min to thereaction temperature (200-325C) and this temperature was keptconstant during the reaction. Reaction of oleic acid with Pt-aluminawas carried out in a similar manner. After the reaction, the catalystparticles were separated, by filtration, from the liquid product andwashed with acetone for further characterizatio |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
< 10 %Spectr. | Stage #1: 1-Iodododecane With Ni{N(SiMe3)(C6H3-2,6-Pri2)}2 In tetrahydrofuran at -35℃; for 0.333333h; Inert atmosphere; Stage #2: methylmagnesium bromide In tetrahydrofuran at 20℃; for 0.75h; Inert atmosphere; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 1-Phenylprop-1-yne; copper dichloride In tetrahydrofuran at 25℃; for 3h; Schlenk technique; Inert atmosphere; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
86 %Chromat. | With buta-1,3-diene; copper dichloride In tetrahydrofuran at 25℃; for 24h; | |
9 %Chromat. | With dicarbonyl(cyclopentadienyl)iron(II) chloride; buta-1,3-diene In tetrahydrofuran at 0 - 20℃; for 24h; Inert atmosphere; Schlenk technique; | Typical procedure for the iron-catalyzed cross-coupling General procedure: To a flame-dried Schlenk tube containing CpFe(CO)2Cl (6) (10.3 mg, 0.05 mmol),3-bromopropyl phenyl ether (1j) (223 mg, 1.04 mmol), THF (0.25 mL), n-BuMgCl (2a)(2M in THF, 0.75 mL, 1.5 mmol), and 1,3-butadiene (90 mL as gas, 4.0 mmol) wereadded successively at -78 C followed by stirring at 0 °C for 2 h and rt for 22 h. Thereaction was quenched by the addition of sat NH4Cl aq., extracted with Et2O (10 mL x3), concentrated, and purified by PTLC (eluent: hexane/Et2O = 99/1) to obtain heptylphenyl etherS2 (3ja) as yellow oil (79.5 mg, 40%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen In acetone at 219.84℃; for 24h; Autoclave; | 2.3. Reaction studies General procedure: Reactions were carried out in a 0.5 L stirred batch autoclavereactor (Autoclave Engineers EZE Seal) equipped with a PID tem-perature controller and a back pressure regulator. The reactor wasloaded with 0.25 Lof a acetone solution of 0.45 g of 1,5-bis(2-furanyl)-1,4-pentadien-3-one (labelled as “A” to better identifiedit) (Alfa Aesar, 98%). Considering the low aqueous solubility of thiscompound, acetone was used as solvent. This solvent was cho-sen taking into account economic reasons as well as the fact thatacetone is already presented in the condensation reaction. Prelim-inary experiments using other solvents, including water and linearalkenes, show very low solubility of the C13 condensation adducts. 70 mg of the catalyst were added (with an average particle diam-eter of 50-80 m) and air was purged out by adding nitrogen upto 1.5 MPa for three times before starting reaction. The C13 loadingand the reactant/catalyst ratio were chosen considering the pre-vious results obtained in the aldolization studies [7]. The reactorwas pressurized to 2.5 MPa of H2, stirred at 1000 rpm and heatedto 493 K, reaching a final pressure of 5.5 MPa. This hydrogen pres-sure is large enough to consider that reaction is carried out in anexcess of hydrogen in comparison to the stoichiometrically needed.According to the theoretic calculations, a complete hydrogenationof all the C13 molecules would imply a consumption of 0.0252 molof H2(0.24 MPa at 293 K). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
21.5% | With 0.5% Pt/Al2O3; hydrogen In acetone at 219.84℃; for 24h; Autoclave; | 2.3. Reaction studies General procedure: Reactions were carried out in a 0.5 L stirred batch autoclavereactor (Autoclave Engineers EZE Seal) equipped with a PID tem-perature controller and a back pressure regulator. The reactor wasloaded with 0.25 Lof a acetone solution of 0.45 g of 1,5-bis(2-furanyl)-1,4-pentadien-3-one (labelled as “A” to better identifiedit) (Alfa Aesar, 98%). Considering the low aqueous solubility of thiscompound, acetone was used as solvent. This solvent was cho-sen taking into account economic reasons as well as the fact thatacetone is already presented in the condensation reaction. Prelim-inary experiments using other solvents, including water and linearalkenes, show very low solubility of the C13 condensation adducts. 70 mg of the catalyst were added (with an average particle diam-eter of 50-80 m) and air was purged out by adding nitrogen upto 1.5 MPa for three times before starting reaction. The C13 loadingand the reactant/catalyst ratio were chosen considering the pre-vious results obtained in the aldolization studies [7]. The reactorwas pressurized to 2.5 MPa of H2, stirred at 1000 rpm and heatedto 493 K, reaching a final pressure of 5.5 MPa. This hydrogen pres-sure is large enough to consider that reaction is carried out in anexcess of hydrogen in comparison to the stoichiometrically needed.According to the theoretic calculations, a complete hydrogenationof all the C13 molecules would imply a consumption of 0.0252 molof H2(0.24 MPa at 293 K). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen; at 400℃; under 750.075 Torr; for 1.0h;Flow reactor; | General procedure: Hydrocarbons were synthesized in a steel flowreactor with an inner diameter of 10 mm. Prior to testing, the FT catalyst as part of the multicomponent bedwas activated in a hydrogen stream supplied at a spacevelocity of 3000 h-1 at 400 and 0.1 MPa for 1 h. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | Stage #1: heptanal With cerium(IV) oxide; water at 450℃; Flow reactor; Stage #2: With Rh/Al2O3; hydrogen at 300℃; Flow reactor; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A Schlenk tube was charged with2 (0.0793 g, 0.271 mmol) and toluene (1.0 mL). A solution of HG2 (0.0085 g, 0.0136mmol, 0.05eq) intoluene (1.0 mL) was added. The mixture was stirred for 2 hours at 100C, and then Pd/C (0.008 g) in ethanol (2 mL) was added. A balloon filled with hydrogen was connected to the Schlenk tube. The mixture was stirred overnight at room temperature. Then the brownish suspension was filtered, the filtrate was analyzed by GC-MS. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72 %Chromat. | With sodium tetrahydroborate; di-tert-butyl peroxide; diphenyldisulfane In <i>tert</i>-butyl alcohol at 120℃; for 48h; Inert atmosphere; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 20% 2: 27% | Stage #1: butyl magnesium bromide With dicarbonyl(cyclopentadienyl)iron(II) chloride; buta-1,3-diene In tetrahydrofuran at 0℃; for 0.166667h; Inert atmosphere; Schlenk technique; Stage #2: 1-Bromononane; methylmagnesium chloride In tetrahydrofuran at 0 - 20℃; for 24h; Inert atmosphere; Schlenk technique; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen In n-heptane at 219.84℃; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 86.7 %Chromat. 2: 4.8 %Chromat. | With hydrogen In decane at 320℃; for 8h; Autoclave; chemoselective reaction; | |
1: 62.8%Chromat. 2: 32.3 %Chromat. | With hydrogen In decane at 280℃; for 8h; Autoclave; | 2.4. Experimental procedure General procedure: The conversion of fatty acids was operated in stainless reactors(50 mL) that purchased from Anhui Kemi Machinery Technology Co.,Ltd. For a typical procedure, stearic acid (0.5 mmol), heterogeneous catalyst (100 mg), and alkane solvent (20 mL) were loaded into a quartzlining in the reactor. The reactor was then purged with hydrogen for three times, and then purged with 4 MPa H2 at room temperature. The reaction was set at reaction temperature for 8 h with a stirring speed of800 rpm. After reaction, the gaseous phase was analyzed by gas chromatography (GC). A Shin Carbon ST 80/100 packed column (Restek) and a thermal conductivity detector (TCD) were used to determine the yields of H2, CO, CO2 and CH4. A Plot Q column and a flame ionization detector (FID) were used to determine the yields of gaseous hydrocarbons such as CH4, C2H6, and C3H8. The liquid products were collected, and eicosane (0.5 mmol) was added as internal standard. The products were analyzed using both gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). GC-MS analysis was conducted by an Agilent 7890B Gas Chromatograph equipped with aHP-5MS 30m ×0.25mm×0.25 μm capillary column (Agilent). The GC was directly interfaced to an Agilent 5977 mass selective detector (EI, 70 eV). A typical GC oven temperature program were listed as follows: 210 °C hold for 2 min, ramp 20 °C min-1 to 300 °C and hold for 2 min. Representative GC spectra are shown in supporting information (Figs. S1 and S2). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Degradation of benzothiophene by synthesized catalysts was studied under UV and visiblelight. To prepare the degradation solution, a predetermined amount of the sample (0.05-0.4 g) was transferred into a degradation cell, and 10 mL of the pollutantsolutions (100-600 mg L-1) was added. The mixture was thoroughly shaken until a homogenous suspension was obtained, and then gently shaken in the dark to maintain the adsorption/desorption process at equilibrium. The mixture was put under UV orvisible light for a predetermined time (0.0-500 min). As UV source, a 30 W, PhilipsHg lamp, and, for visible light, a 30 W fluorescence lamp were used. The lamps were installed 10 cm above the cell [15, 16]. After irradiation, the photocatalyst was removedand the benzothiophene content was measured at lambdamax = 246 nm. Blank samples (without photocatalysts) were used to evaluate the rate of photolysis of the pollutants. The degradation efficiency was determined by Eq. (1):% Degradation = ((A0 - At)/A0)x100 A0 and At are the absorbance of pollutant before and after irradiation, respectively.The effect of different influencing variables including ZnO content of the photocatalyst,irradiation time, pollutant initial concentration, catalyst dose, and the effect of H2O2 on pollutant decomposition was studied. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With iron(II) bis(trimethylsilyl)amide; hydrogen; diisobutylaluminium hydride at 20℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 67.3 %Chromat. 2: 28.2 %Chromat. | With hydrogen In decane at 280℃; for 8h; Autoclave; | 2.4. Experimental procedure General procedure: The conversion of fatty acids was operated in stainless reactors(50 mL) that purchased from Anhui Kemi Machinery Technology Co.,Ltd. For a typical procedure, stearic acid (0.5 mmol), heterogeneous catalyst (100 mg), and alkane solvent (20 mL) were loaded into a quartzlining in the reactor. The reactor was then purged with hydrogen for three times, and then purged with 4 MPa H2 at room temperature. The reaction was set at reaction temperature for 8 h with a stirring speed of800 rpm. After reaction, the gaseous phase was analyzed by gas chromatography (GC). A Shin Carbon ST 80/100 packed column (Restek) and a thermal conductivity detector (TCD) were used to determine the yields of H2, CO, CO2 and CH4. A Plot Q column and a flame ionization detector (FID) were used to determine the yields of gaseous hydrocarbons such as CH4, C2H6, and C3H8. The liquid products were collected, and eicosane (0.5 mmol) was added as internal standard. The products were analyzed using both gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). GC-MS analysis was conducted by an Agilent 7890B Gas Chromatograph equipped with aHP-5MS 30m ×0.25mm×0.25 μm capillary column (Agilent). The GC was directly interfaced to an Agilent 5977 mass selective detector (EI, 70 eV). A typical GC oven temperature program were listed as follows: 210 °C hold for 2 min, ramp 20 °C min-1 to 300 °C and hold for 2 min. Representative GC spectra are shown in supporting information (Figs. S1 and S2). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With hydrogen at 200℃; for 24h; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water-d2 at 20℃; for 1h; Sonication; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With whole cells of Escherichia coli overexpressed short-length Chlorella variabillis photodecarboxylase In dimethyl sulfoxide at 30℃; for 6h; Sealed tube; Irradiation; Microbiological reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97.4% | With hydrogen In cyclohexane at 300℃; for 6h; | 2.3. Catalytic deoxygenation General procedure: The catalytic deoxygenation of MO, JO and WCO using fresh NiCeAlcatalysts were conducted using a stirred batch reactor [YZPR-100(M),YanZheng Instrument, Shanghai, China] with a maximum operatingpressure of 15 MPa at 400 . In each experiment, after the reactor waspurged with pure N2 at least 3 times at room temperature, 0.1 g catalystand 1 g reactant were introduced into the reactor which then was slowlyheated to reaction temperature (300 ). Then 2.5 MPa H2 was introducedto initiate the catalytic deoxygenation reaction for 6 h. In order toreduce the error and contingency during test, all experiments wererepeated at least three times to ensure the accuracy of the data. Recyclabilitytest and deoxygenation experiments using fresh, spent and regenerated NiCeAl-3.0 were also performed at the same conditiondescribed above |
Tags: 629-50-5 synthesis path| 629-50-5 SDS| 629-50-5 COA| 629-50-5 purity| 629-50-5 application| 629-50-5 NMR| 629-50-5 COA| 629-50-5 structure
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Code | Phrase |
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Code | Phrase |
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P378 | |
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P391 | Collect spillage. Hazardous to the aquatic environment |
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Code | Phrase |
P401 | |
P402 | Store in a dry place. |
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Code | Phrase |
H200 | Unstable explosive |
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H260 | In contact with water releases flammable gases which may ignite spontaneously |
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Health hazards | |
Code | Phrase |
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H305 | May be harmful if swallowed and enters airways |
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H311 | Toxic in contact with skin |
H312 | Harmful in contact with skin |
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H316 | Causes mild skin irritation |
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H318 | Causes serious eye damage |
H319 | Causes serious eye irritation |
H320 | Causes eye irritation |
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H351 | Suspected of causing cancer |
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H361d | Suspected of damaging the unborn child |
H362 | May cause harm to breast-fed children |
H370 | Causes damage to organs |
H371 | May cause damage to organs |
H372 | Causes damage to organs through prolonged or repeated exposure |
H373 | May cause damage to organs through prolonged or repeated exposure |
Environmental hazards | |
Code | Phrase |
H400 | Very toxic to aquatic life |
H401 | Toxic to aquatic life |
H402 | Harmful to aquatic life |
H410 | Very toxic to aquatic life with long-lasting effects |
H411 | Toxic to aquatic life with long-lasting effects |
H412 | Harmful to aquatic life with long-lasting effects |
H413 | May cause long-lasting harmful effects to aquatic life |
H420 | Harms public health and the environment by destroying ozone in the upper atmosphere |
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