* 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.
In N,N-dimethyl-formamide; at 110℃; for 15h;Inert atmosphere;
A mixture of tripropylamine (1 mol) and propyl bromide (1.5 mol) in DMF (100mL) was stirred at 110 C for 15 h under an N2 atmosphere. After completion of reaction, the reaction mixture was cooled (ice-bath) and n-hexane/toluene (2 : 1)(200 mL) was added. The precipitate was filtered and washed with n-hexane/toluene (3 : 1) (40 mL) to give the desired TPAB
EXAMPLE 8 The procedure of Example 1 was repeated, except that 8.7 g (0.033 mol) of tetra-n-propyl ammonium bromide was used in the place of tetraethyl ammonium bromide. The resultant reaction solution was subjected to after-treatment. When the organic layer consequently obtained was analyzed by gas chromatography, it was found to contain 111.4 g (0.674 mol) of 3-cyano-3,5,5-trimethyl cyclohexane and 40.4 g of an unaltered isophorone. Thus, the yield of 3-cyano-3,5,5-trimethyl cyclohexanone (based on hydrogen cyanide) was 96% and the selectivity of the reaction (based on the converted isophorone) was 95%.
With hydrogenchloride; sodium hydroxide; In water;
EXAMPLE 8 30.6 g of 2,2'-dithiodibenzoic acid (0.10 mol) are introduced into and dissolved in a solution of 8.00 g of sodium hydroxide (0.20 mol) in 800 ml of water at room temperature, while stirring. A solution of 26.6 g of <strong>[1941-30-6]tetrapropylammonium bromide</strong> (0.10 mol) in 300 ml of water is added to this solution. A solution of 3.65 g of hydrogen chloride (0.10 mol) in 100 ml of water is then slowly added dropwise, during which the product precipitates. The reaction mixture is subsequently stirred for 15 hours. The precipitate is then filtered off with suction, washed with water and dried in a through-circulation drying cabinet at 120 C. Yield: 48.3 g (98.2% of theory) of 2,2'-dithiodibenzoic acid mono(tetrapropylammonium) salt of the formula shown in Example 5.
EXAMPLE 1 135 g (1.09 moles) of propyl bromide and 140 g (0.96 moles) of tripropylamine are heated together with 200 ml of dimethylformamide up to 130 C., in equipment provided with reflux condenser and thermometer, for 6 hours. The end point can be ascertained by the disappearance of the two phases formed from propyl bromide and dimethylformamide/tripropylamine and by the rise in temperature. The resulting solution is cooled and crystals of tetrapropylammonium bromide are precipitated. The crystalline product is filtered and dried. Yield: 162 g (63% in reference to the tripropylamine).
With tri-n-propylamine;
EXAMPLE 2 135 g (1.09 moles) of propylbromide and 140 g (0.96 moles) of tripropylamine are combined with the mother liquor of Example 1 and are heated again for 6 hours to 130 C. Upon cooling the solution, crystals of tetrapropylammonium bromide precipitated. Yield: 174 g (65% referred to the tripropylamine). This mother liquor can be further used. By concentrating the mother liquor down to half the volume, another 50.8 g (19% in reference to tripropylamine) of tetrapropylammonium bromide can be isolated from the mother liquor.
With tri-n-propylamine; In nitromethane;
EXAMPLE 5 125 g (1 mole) of propyl bromide and 140 g (0.96 moles) of tripropylamine are heated together with 200 ml of nitromethane with stirring for 12 hours at 50 C. Upon cooling the resulting solution, crystals of tetrapropylammonium bromide precipitated.
bis(tetrapropylammonium) tetrathiotungstate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With ammonium tetrathiotungstate; In water;
For the synthesizing method of tetrapropylammonium tetrathiotungstate [(Pr4N)2WS4] as a photocatalyst precursor, a solution of ammonium tetrathiotungstate [(NH4)2WS4] is reacted with an aqueous solution of tetraproplyammonium bromide [(Pr4N)Br] to produce an orange-yellow micro-crystalline solid. The chemical reaction which involved is shown as below:2[(Pr4N)Br] + [(NH4)2WS4] > [(Pr4N)2WS4] + 2[(NH4)Br]The orange-yellow micro-crystalline solid which acted as a precipitate will be filtered, washed with diethyl ether and then dried. As for the synthesizing method of tris(l- carboxyl-2-phenyl-l,2-ethylenodithiolenic-S,S') tungsten complex [CaYHi8O2S6W], a solution of the precursor [(Pr4N)2WS4] will be reacted with a solution of phenylacetylenecarboxylate [C9H6O2]. Dried acetonitrile will also be used in this reaction. The solution mixture is purified by using a LH-20 column chromatography and eluted with acetonitrile-benzene to give several fractions. Evaporation of solvent from the solution mixture will give a dark brown solid of the tris(l-carboxyl-2- phenyl-l,2-ethylenodithiolenic-S,S') tungsten complex.
With potassium hydroxide; In ethanol; at 40℃; for 12h;Inert atmosphere;
1) Synthesis of Tetrapropyl Ammonium Hydroxide Ethanol Solution:<strong>[1941-30-6]Tetrapropylammonium bromide</strong> (2.7 g, 10 mmol) was placed50 mL of the reaction flask,The reaction flask was evacuated through nitrogen three times,Was added under nitrogenThe distilled ethanolic solution (10 mL),40oC conditions for 10min,KOH solid (0.62 g, 11 mmol) was added,Reaction 12h, the exchange completely filtered,The filtrate was allowed to stand at low temperature for 6 hours under nitrogen atmosphere,And then precipitated solid filter, so repeated 3 times, Can be obtainedTetrapropylammonium hydroxide in ethanol.
With bromine; for 0.5h;Schlenk technique; Inert atmosphere;
This procedure can be also used for the in situ preparation of Pr4NBr9. A flame-dried, argon-backfilled Schlenk tube equipped with a magnetic stir bar and a rubber septum was charged with Pr4NBr (532.5 mg, 2.0 mmol, 1 equiv) followed by slow addition of Br2 (430.4 muL, 8.4 mmol, 4.2 equiv). The mixture was stirred for 30 min and became a homogeneous dark-red liquid. Stirring was ceased and the reaction vessel was cooled to 4 C for ca. 10 min after which the mixture became solid and remained solid after rewarming to r.t.; yield: 1.79 g (99%). Raman analysis of the reagent prepared this way showed that Pr4NBr9 was the only species present in the solid. The reagent was transferred to a screw-cap vial and remained stable for several weeks as long as the vial was correctly sealed. Under reduced pressure the compound released bromine and decayed to the tribromide.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
General procedure: The DESs were prepared with TPAB as the organic salt. The HBD used were ethylene glycol, triethylene glycol and glycerol. The TPAB:HBD of molar ratios 1:3, 1:4, and 1:5 were used. In the case of TPAB:triethylene glycol the ratios were 1:2.5, 1:3, and 1:4. DES samples synthesized in different TPAB/HBD molar ratios are shown in Table 1. An incubator shaker (Brunswick Scientific Model INNOVA 40R) was used to mix the salt and the HBD. Each DES mixture was mixed at 400 rpm and 353.15 K for 2 h until a homogeneous transparent colorless liquid was formed. DES samples were synthesized at atmospheric pressure and under tight control of moisture content. Samples were kept in well sealed glass vials after preparation and fresh samples were used for analysis to avoid structural change or environmental effects on their physical properties. The properties measured were density, viscosity, surface tension, conductivity, reflective index and pH. The temperature range considered for all measured physical properties was 293.15-353.15 K.
The organic-inorganic hybrid catalysts were prepared by adding drop wise, the required amount of aq. 1 M solution of (C3H7)4N+Br to aqueous solution of HPA hydrates (PWA, SWA, PMoA) (0.02 M)at room temperature with stirring. The obtained slurry containing precipitate was stirred for 2 h, filtered, washed with water and dried in an oven at 120 C for 4 h and activated at 150 C before use. The catalysts were designated as (C3H7)4N+/PWA,(C3H7)4N+/SWA, (C3H7)4N+/PMoA for respective HPAs. Different organic salts on PWA were prepared by following the same procedure as mentioned above by varying the organic salt and are designated as C8H20N+/PWA and C19H42N+/PWA. Cs/PWA andNH4/PWA catalysts were prepared by literature methods [29,30 ]and other solid acid catalysts were activated at 150C prior to the reaction.
General procedure: The organic-inorganic hybrid catalysts were prepared by adding drop wise, the required amount of aq. 1 M solution of (C3H7)4N+Br to aqueous solution of HPA hydrates (PWA, SWA, PMoA) (0.02 M)at room temperature with stirring. The obtained slurry containing precipitate was stirred for 2 h, filtered, washed with water and dried in an oven at 120 C for 4 h and activated at 150 C before use. The catalysts were designated as (C3H7)4N+/PWA,(C3H7)4N+/SWA, (C3H7)4N+/PMoA for respective HPAs. Different organic salts on PWA were prepared by following the same procedure as mentioned above by varying the organic salt and are designated as C8H20N+/PWA and C19H42N+/PWA. Cs/PWA andNH4/PWA catalysts were prepared by literature methods [29,30 ]and other solid acid catalysts were activated at 150C prior to the reaction.
General procedure: The organic-inorganic hybrid catalysts were prepared by adding drop wise, the required amount of aq. 1 M solution of (C3H7)4N+Br to aqueous solution of HPA hydrates (PWA, SWA, PMoA) (0.02 M)at room temperature with stirring. The obtained slurry containing precipitate was stirred for 2 h, filtered, washed with water and dried in an oven at 120 C for 4 h and activated at 150 C before use. The catalysts were designated as (C3H7)4N+/PWA,(C3H7)4N+/SWA, (C3H7)4N+/PMoA for respective HPAs. Different organic salts on PWA were prepared by following the same procedure as mentioned above by varying the organic salt and are designated as C8H20N+/PWA and C19H42N+/PWA. Cs/PWA andNH4/PWA catalysts were prepared by literature methods [29,30 ]and other solid acid catalysts were activated at 150C prior to the reaction.
bis(fluorosulfonyl)imide tetrapropylammonium salt[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With potassium bis(fluorosulfuryl)amide; In water;
Two hundred grams of the final reaction solution prepared as described in the Example 1 was dissolved in 800 g of water. Then, the solution was neutralized with 52 g of potassium carbonate, having the pH of the solution increased to 7. The precipitated fluorosulfate potassium salt was filtered out. Then, an aqueous solution dissolving 37 g of <strong>[1941-30-6]tetrapropylammonium bromide</strong> was dripped into the filtered neutralized solution. Once the dripping started, crystals of bis(fluorosulfonyl)imide tetrapropylammonium salt were precipitated out. After recovering the precipitated crystals by filtration, they were dried in a drier set at 60 C. In this way, 48 g of bis(fluorosulfonyl)imide tetrapropylammonium salt was obtained (the recovery based on the precursor urea was 30%). The content of the fluoride ion in the obtained bis(fluorosulfonyl)imide tetrapropylammonium salt was 1 ppm. The boiling point of the obtained sample was 140 to 141 C.
[Cd(1,3,5-benzenetricarboxylate)(N,N-dimethylformamide)](tetrapropylammonium)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With 1,4-diaza-bicyclo[2.2.2]octane; In water; at 80℃; for 72h;
Reaction mixture of Cd(CH3COO)2·2H2O (0.1770g, 0.6mmol) and H3BTC (0.0637g, 0.3mmol), l-alanine (0.0267g, 0.3mmol), 1,4-diazabicyclo-[2.2.2]octane (DBO, 0.0363g, 0.3mmol) and N(Pr)4·Br (0.0176g, 0.066mmol) in 3mL DMF and 2mL H2O was placed in a 20mL vial. The sample was stirred for 20min and heated at 80C for 3 days. Colorless block crystals of 1 were isolated by filtration and washed by DMF.
Reaction of carbazole with 4,5-difluorophthalonitrile affords intermediate 15 which on hydrolysis provides potassium salt of the dicarboxylic acid 16. Reaction with 14 n-Pr4NBr affords the product XXI. A similar approach using 15 3,6-di-tert-butyl-9H-carbazole 17 affords the intermediate 18 on reaction with 11 4,5-difluorophthalonitrile. Hydrolysis provides the 12 potassium salt of the dicarboxylic acid XXII. Conversion to the product XXIII is made by reaction with n-Pr4NBr.
C12H28N(1+)*Fe(2+)*0.29Fe(3+)*0.71V(3+)*3C2O2S2(2-)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With ascorbic acid; In water; for 1h;
General procedure: The precursor K2(dto) was prepared according to the literature [32]. All other reagents and solvents were commercial-grade reagents and used without further purification.(n-C3H7)4N[FeIIFeIII1-xVIIIx(dto)3] were prepared by the following synthesis method. A solution containing FeCl2·4H2O (0.5mmol), (n-C3H7)4NBr (0.5mmol) and ascorbic acid (10mg) in a water was stirred. To this, a solution containing VCl3 (× mmol), FeCl3·9H2O (0.5-× mmol) and K2(dto) (300mg, 1.5mmol) in a water was added dropwise then stirred the mixture solution for one hour. Black powdered sample was precipitated, collected by suction filtration, and washed with methanol and water before dried in vacuo.
C12H28N(1+)*Fe(2+)*0.15Fe(3+)*0.85V(3+)*3C2O2S2(2-)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With ascorbic acid; In water; for 1h;
General procedure: The precursor K2(dto) was prepared according to the literature [32]. All other reagents and solvents were commercial-grade reagents and used without further purification.(n-C3H7)4N[FeIIFeIII1-xVIIIx(dto)3] were prepared by the following synthesis method. A solution containing FeCl2·4H2O (0.5mmol), (n-C3H7)4NBr (0.5mmol) and ascorbic acid (10mg) in a water was stirred. To this, a solution containing VCl3 (× mmol), FeCl3·9H2O (0.5-× mmol) and K2(dto) (300mg, 1.5mmol) in a water was added dropwise then stirred the mixture solution for one hour. Black powdered sample was precipitated, collected by suction filtration, and washed with methanol and water before dried in vacuo.
C12H28N(1+)*Fe(2+)*0.06Fe(3+)*0.94V(3+)*3C2O2S2(2-)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With ascorbic acid; In water; for 1h;
General procedure: The precursor K2(dto) was prepared according to the literature [32]. All other reagents and solvents were commercial-grade reagents and used without further purification.(n-C3H7)4N[FeIIFeIII1-xVIIIx(dto)3] were prepared by the following synthesis method. A solution containing FeCl2·4H2O (0.5mmol), (n-C3H7)4NBr (0.5mmol) and ascorbic acid (10mg) in a water was stirred. To this, a solution containing VCl3 (× mmol), FeCl3·9H2O (0.5-× mmol) and K2(dto) (300mg, 1.5mmol) in a water was added dropwise then stirred the mixture solution for one hour. Black powdered sample was precipitated, collected by suction filtration, and washed with methanol and water before dried in vacuo.
C12H28N(1+)*Fe(2+)*0.79Fe(3+)*0.21V(3+)*3C2O2S2(2-)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With ascorbic acid; In water; for 1h;
General procedure: The precursor K2(dto) was prepared according to the literature [32]. All other reagents and solvents were commercial-grade reagents and used without further purification.(n-C3H7)4N[FeIIFeIII1-xVIIIx(dto)3] were prepared by the following synthesis method. A solution containing FeCl2·4H2O (0.5mmol), (n-C3H7)4NBr (0.5mmol) and ascorbic acid (10mg) in a water was stirred. To this, a solution containing VCl3 (× mmol), FeCl3·9H2O (0.5-× mmol) and K2(dto) (300mg, 1.5mmol) in a water was added dropwise then stirred the mixture solution for one hour. Black powdered sample was precipitated, collected by suction filtration, and washed with methanol and water before dried in vacuo.
C12H28N(1+)*Fe(2+)*0.66Fe(3+)*0.34V(3+)*3C2O2S2(2-)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With ascorbic acid; In water; for 1h;
General procedure: The precursor K2(dto) was prepared according to the literature [32]. All other reagents and solvents were commercial-grade reagents and used without further purification.(n-C3H7)4N[FeIIFeIII1-xVIIIx(dto)3] were prepared by the following synthesis method. A solution containing FeCl2·4H2O (0.5mmol), (n-C3H7)4NBr (0.5mmol) and ascorbic acid (10mg) in a water was stirred. To this, a solution containing VCl3 (× mmol), FeCl3·9H2O (0.5-× mmol) and K2(dto) (300mg, 1.5mmol) in a water was added dropwise then stirred the mixture solution for one hour. Black powdered sample was precipitated, collected by suction filtration, and washed with methanol and water before dried in vacuo.
C12H28N(1+)*Fe(2+)*0.48Fe(3+)*0.52V(3+)*3C2O2S2(2-)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With ascorbic acid; In water; for 1h;
General procedure: The precursor K2(dto) was prepared according to the literature [32]. All other reagents and solvents were commercial-grade reagents and used without further purification.(n-C3H7)4N[FeIIFeIII1-xVIIIx(dto)3] were prepared by the following synthesis method. A solution containing FeCl2·4H2O (0.5mmol), (n-C3H7)4NBr (0.5mmol) and ascorbic acid (10mg) in a water was stirred. To this, a solution containing VCl3 (× mmol), FeCl3·9H2O (0.5-× mmol) and K2(dto) (300mg, 1.5mmol) in a water was added dropwise then stirred the mixture solution for one hour. Black powdered sample was precipitated, collected by suction filtration, and washed with methanol and water before dried in vacuo.
General procedure: The precursor K2(dto) was prepared according to the literature [32]. All other reagents and solvents were commercial-grade reagents and used without further purification.(n-C3H7)4N[FeIIFeIII1-xVIIIx(dto)3] were prepared by the following synthesis method. A solution containing FeCl2·4H2O (0.5mmol), (n-C3H7)4NBr (0.5mmol) and ascorbic acid (10mg) in a water was stirred. To this, a solution containing VCl3 (× mmol), FeCl3·9H2O (0.5-× mmol) and K2(dto) (300mg, 1.5mmol) in a water was added dropwise then stirred the mixture solution for one hour. Black powdered sample was precipitated, collected by suction filtration, and washed with methanol and water before dried in vacuo.
With sodium tungstate (VI) dihydrate; HO4P(2-)*Na(1+)*12H2O;pH 2.8 - 3.4;
General procedure: The POTVs were synthesized according to the literature data [53].NaHPO4·12H2O (0.025 mol) was added to an aqueous solution ofNa2WO4·2H2O (0.019 mol) under continuous stirring, and the pH wasadjusted with HCl (36% v/v) to 2.8. After stirring, 3.75 ml (PVW) or5.00 ml (PV2W) of vanadium stock solution was added dropwise. Theorange color solution was acidified with concentrated HCl to adjust thepH up to 3.4. The organic salts of POTVs were obtained by the additionof 0.012 mol of <strong>[1941-30-6]tetrapropylammonium bromide</strong>. The yellow (PVW) ororange (PV2W) solid formed was filtered and dried under vacuum untilconstant weight. Vanadium (V) stock solution was prepared by mixingNH4VO3 (0.25 mol) with NaOH (0.50 mol) in 500 ml of distilled water.
With sodium tungstate (VI) dihydrate; HO4P(2-)*Na(1+)*12H2O;pH 2.8 - 3.4;
General procedure: The POTVs were synthesized according to the literature data [53].NaHPO4·12H2O (0.025 mol) was added to an aqueous solution ofNa2WO4·2H2O (0.019 mol) under continuous stirring, and the pH wasadjusted with HCl (36% v/v) to 2.8. After stirring, 3.75 ml (PVW) or5.00 ml (PV2W) of vanadium stock solution was added dropwise. Theorange color solution was acidified with concentrated HCl to adjust thepH up to 3.4. The organic salts of POTVs were obtained by the additionof 0.012 mol of <strong>[1941-30-6]tetrapropylammonium bromide</strong>. The yellow (PVW) ororange (PV2W) solid formed was filtered and dried under vacuum untilconstant weight. Vanadium (V) stock solution was prepared by mixingNH4VO3 (0.25 mol) with NaOH (0.50 mol) in 500 ml of distilled water.