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CAS No. : | 19094-56-5 | MDL No. : | MFCD00079731 |
Formula : | C7H4ClIO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | GEBYSTBEDVQOTK-UHFFFAOYSA-N |
M.W : | 282.46 | Pubchem ID : | 519638 |
Synonyms : |
|
Num. heavy atoms : | 11 |
Num. arom. heavy atoms : | 6 |
Fraction Csp3 : | 0.0 |
Num. rotatable bonds : | 1 |
Num. H-bond acceptors : | 2.0 |
Num. H-bond donors : | 1.0 |
Molar Refractivity : | 51.13 |
TPSA : | 37.3 Ų |
GI absorption : | High |
BBB permeant : | Yes |
P-gp substrate : | No |
CYP1A2 inhibitor : | No |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -6.02 cm/s |
Log Po/w (iLOGP) : | 1.63 |
Log Po/w (XLOGP3) : | 2.82 |
Log Po/w (WLOGP) : | 2.64 |
Log Po/w (MLOGP) : | 3.09 |
Log Po/w (SILICOS-IT) : | 2.83 |
Consensus Log Po/w : | 2.6 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 0.0 |
Bioavailability Score : | 0.56 |
Log S (ESOL) : | -3.71 |
Solubility : | 0.0556 mg/ml ; 0.000197 mol/l |
Class : | Soluble |
Log S (Ali) : | -3.26 |
Solubility : | 0.155 mg/ml ; 0.000549 mol/l |
Class : | Soluble |
Log S (SILICOS-IT) : | -3.33 |
Solubility : | 0.131 mg/ml ; 0.000465 mol/l |
Class : | Soluble |
PAINS : | 0.0 alert |
Brenk : | 1.0 alert |
Leadlikeness : | 0.0 |
Synthetic accessibility : | 1.7 |
Signal Word: | Danger | Class: | 6.1 |
Precautionary Statements: | P273-P280-P301+P310+P330-P305+P351+P338+P310 | UN#: | 2811 |
Hazard Statements: | H301-H318-H400 | 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 |
---|---|---|
93.7% | Stage #1: With sulfuric acid; sodium nitrite In water at 0 - 10℃; Stage #2: With urea; potassium iodide In water at 0℃; for 0.5 h; |
123 g of 2-chloro-5-aminobenzoic acid was added to 2000 g of a 20percent aqueous solution of sulfuric acid, and the temperature was maintained at 0 to 10 ° C. An aqueous solution of sodium nitrite (51 g of sodium nitrite dissolved in 200 g of water) was added dropwise, The reaction solution was solid, TLC (PE / EA: 1/3). After the reaction was completed, 1.2 g of urea was added, cooled to 0 ° C with stirring, and potassium iodide solution (130 g of KI dissolved in 500 g of water) was rapidly added,Stir until no bubbles continue to stir for 30min, filter, 200g washed to get brown solid;The solid was dissolved in 400 g of ethyl acetate, washed with 300 ml of 1N hydrochloric acid,300 ml of 10percent sodium hydrogen sulfate, 400 ml of saturated brine, dried over magnesium sulfate, dried at 50 ° C under reduced pressure to obtain a crude product, and 400 ml of toluene was added at 80 ° C for 1 h,Cooling 0 ~ 5° C crystallization 1h, pumping 50° C under reduced pressure drying,To give a pale yellow solid2-chloro-5-iodobenzoic acid 191 g was 99.6percent pure and the yield was 93.7percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94% | at 25 - 30℃; for 5 h; | Example 1 : Synthesis of the fluoride VIII.1Oxalylchloride (176kg; 1386mol; 1 ,14eq) is added to a mixture of 2-chloro-5-iodo benzoic acid (343kg; 1214mol) (compound IX.1 ), fluorobenzene (858kg) and N,N- dimethylformamide (2kg) within 3 hours at a temperature in the range from about 25 to 30°C (gas formation). After completion of the addition, the reaction mixture is stirred for additional 2 hours at a temperature of about 25 to 30°C. The solvent (291 kg) is distilled off at a temperature between 40 and 45°C (p=200mbar). Then the reaction solution (91 1 kg) is added to aluminiumchloride AICI3 (181 kg) andfluorobenzene (192kg) at a temperature between about 25 and 30°C within 2 hours. The reaction solution is stirred at the same temperature for about an additional hour. Then the reaction mixture is added to an amount of 570 kg of water within about 2 hours at a temperature between about 20 and 30°C and stirred for an additional hour. After phase separation the organic phase (1200kg) is separated into two halves (600kg each). From the first half of the organic phase solvent (172kg) is distilled off at a temperature of about 40 to 50°C (p=200mbar). Then 2-propanole (640kg) is added. The solution is heated to about 50°C and then filtered through a charcoal cartouche (clear filtration). The cartouche may be exchanged during filtration and washed with a fluorobenzene/2-propanole mixture (1 :4; 40kg) after filtration. Solvent (721 kg) is distilled off at a temperature of about 40 to 50°C and p=200mbar. Then 2-propanole (240kg) is added at a temperature in the range between about 40 to 50°C. If the content of fluorobenzene is greater than 1 percent as determined via GC, another 140kg of solvent are distilled off and 2-propanole (140kg) is added. Then the solution is cooled from about 50°C to 40°C within one hour and seeding crystals (50g) are added. The solution is further cooled from about 40°C to 20°C within 2 hours. Water (450kg) is added at about 20°C within 1 hour and the suspension is stirred at about 20°C for an additional hour before the suspension is filtered. The filter cake is washed with 2-propanole/water (1 :1 ; 800kg). The product is dried until a water level of <0.06percentw/w is obtained. The second half of the organic phase is processed identically. A total of 410kg (94percentyield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. |
94% | Stage #1: With oxalyl dichloride In N,N-dimethyl-formamide at 25 - 30℃; for 5 h; Stage #2: at 20 - 30℃; for 6 h; |
Oxalylchloride (176 kg; 1386 mol; 1.14 eq) is added to a mixture of 2-chloro-5-iodo benzoic acid (343 kg; 1214 mol) (compound IX.1), fluorobenzene (858 kg) and N,N-dimethylformamide (2 kg) within 3 hours at a temperature in the range from about 25 to 30° C. (gas formation). After completion of the addition, the reaction mixture is stirred for additional 2 hours at a temperature of about 25 to 30° C. The solvent (291 kg) is distilled off at a temperature between 40 and 45° C. (p=200 mbar). Then the reaction solution (911 kg) is added to aluminiumchloride AlCl3 (181 kg) and fluorobenzene (192 kg) at a temperature between about 25 and 30° C. within 2 hours. The reaction solution is stirred at the same temperature for about an additional hour. Then the reaction mixture is added to an amount of 570 kg of water within about 2 hours at a temperature between about 20 and 30° C. and stirred for an additional hour. After phase separation the organic phase (1200 kg) is separated into two halves (600 kg each). From the first half of the organic phase solvent (172 kg) is distilled off at a temperature of about 40 to 50° C. (p=200 mbar). Then 2-propanole (640 kg) is added. The solution is heated to about 50° C. and then filtered through a charcoal cartouche (clear filtration). The cartouche may be exchanged during filtration and washed with a fluorobenzene/2-propanole mixture (1:4; 40 kg) after filtration. Solvent (721 kg) is distilled off at a temperature of about 40 to 50° C. and p=200 mbar. Then 2-propanole (240 kg) is added at a temperature in the range between about 40 to 50° C. If the content of fluorobenzene is greater than 1percent as determined via GC, another 140 kg of solvent are distilled off and 2-propanole (140 kg) is added. Then the solution is cooled from about 50° C. to 40° C. within one hour and seeding crystals (50 g) are added. The solution is further cooled from about 40° C. to 20° C. within 2 hours. Water (450 kg) is added at about 20° C. within 1 hour and the suspension is stirred at about 20° C. for an additional hour before the suspension is filtered. The filter cake is washed with 2-propanole/water (1:1; 800 kg). The product is dried until a water level of <0.06percent w/w is obtained. The second half of the organic phase is processed identically. A total of 410 kg (94percent yield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. |
94% | With aluminum (III) chloride; oxalyl dichloride In N,N-dimethyl-formamide at 25 - 45℃; Industry scale | Oxalylchloride (176 kg; 1386 mol; 1.14 eq) is added to a mixture of 2-chloro-5-iodo benzoic acid (343 kg; 1214 mol) (compound IX.1), fluorobenzene (858 kg) and N,N-dimethylformamide (2 kg) within 3 hours at a temperature in the range from about 25 to 30° C. (gas formation). After completion of the addition, the reaction mixture is stirred for additional 2 hours at a temperature of about 25 to 30° C. The solvent (291 kg) is distilled off at a temperature between 40 and 45° C. (p=200 mbar). Then the reaction solution (911 kg) is added to aluminiumchloride AlCl3 (181 kg) and fluorobenzene (192 kg) at a temperature between about 25 and 30° C. within 2 hours. The reaction solution is stirred at the same temperature for about an additional hour. Then the reaction mixture is added to an amount of 570 kg of water within about 2 hours at a temperature between about 20 and 30° C. and stirred for an additional hour. After phase separation the organic phase (1200 kg) is separated into two halves (600 kg each). From the first half of the organic phase solvent (172 kg) is distilled off at a temperature of about 40 to 50° C. (p=200 mbar). Then 2-propanole (640 kg) is added. The solution is heated to about 50° C. and then filtered through a charcoal cartouche (clear filtration). The cartouche may be exchanged during filtration and washed with a fluorobenzene/2-propanole mixture (1:4; 40 kg) after filtration. Solvent (721 kg) is distilled off at a temperature of about 40 to 50° C. and p=200 mbar. Then 2-propanole (240 kg) is added at a temperature in the range between about 40 to 50° C. If the content of fluorobenzene is greater than 1percent as determined via GC, another 140 kg of solvent are distilled off and 2-propanole (140 kg) is added. Then the solution is cooled from about 50° C. to 40° C. within one hour and seeding crystals (50 g) are added. The solution is further cooled from about 40° C. to 20° C. within 2 hours. Water (450 kg) is added at about 20° C. within 1 hour and the suspension is stirred at about 20° C. for an additional hour before the suspension is filtered. The filter cake is washed with 2-propanole/water (1:1; 800 kg). The product is dried until a water level of <0.06percent w/w is obtained. The second half of the organic phase is processed identically. A total of 410 kg (94percent yield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. |
78.6% | Stage #1: With oxalyl dichloride; N,N-dimethyl-formamide In dichloromethane for 3 h; Stage #2: With aluminum (III) chloride In dichloromethane at 0 - 5℃; for 1 h; |
5-Iodo-2-chlorobenzoic acid (20.0 g, 0.071 mol) was added to a solution of 2.0 M oxalyl chloride in dichloromethane (39 ml, 0.078 mol), stirred for suspension, and then 8 drops of DMF solution was added dropwise. After the reaction was carried out for 3 hours, the solution was clarified and the reaction was almost complete. The solvent was spin-dried on a rotary evaporator, then 15 ml of methylene chloride was added, and the solvent was dried. After spin-drying, add 30 ml of dichloromethane, stir, cool to 0-5 ° C, add fluorobenzene (7. lg, 0.074 mol), add anhydrous aluminum trichloride (9.9 g, 0.074 mol) in batches, control The temperature is not more than 5 °C, after the completion of the addition, stirring is continued at 4 ° C for 1 h, the reaction is almost complete by TLC, the reaction is quenched on ice-water mixture, the organic phase is separated, and the aqueous phase is extracted with dichloromethane. The phase was washed twice with 1 mol/L hydrochloric acid, washed once with water, and washed twice with 1 mol/L NaOH solution.The mixture was washed twice with saturated sodium chloride and dried over anhydrous sodium sulfate. Drain filtration, spin dry solvent to obtain oilAfter column chromatography, 20. 1g (78.6percent) of a white solid was obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
73.74% | Stage #1: With oxalyl dichloride In dichloromethane; N,N-dimethyl-formamide at 25 - 30℃; for 1 h; Stage #2: With aluminum (III) chloride In dichloromethane; N,N-dimethyl-formamide at -15 - -5℃; for 0.5 h; Stage #3: at -10 - -5℃; for 2 h; |
Charged 2-chloro-5-iodobenzoic acid (200 gm, 0.7080 moles), dichloromethane(1000 ml) and N,N-dimethylformamide (5 ml) at 25°C to 30°C. Under stirring slowly charged oxalyl chloride (107.9 gm, 0.8496 moles) and maintained stirring for one hour. Applied cooling and cooled the reaction mass to -15°C to -10°C. Charged aluminum chloride (113.29gm, 0.8496 moles) maintaining the reaction mass temperature at -10°C to -5°C and stirred for 30 minutes. Charged phenatole (86.49gm, 0.7080 moles) to the reaction mixture and maintained under stirring for 2 hours at -10°C to -5°C. The progress of the reaction was monitored by HPLC. After completion of the reaction the reaction mixture was quenched by adding water and dilute hydrochloric acid. Raised the temperature of the reaction mixture to 25°C to 30°C and maintained for 30 minutes. Separated the organic layer, extracted the aqueous layer again with dichloromethane (400 ml). The combined organic layer was washed with 10percent of sodium bicarbonate solution (600 ml) followed with 5percent brine solution (600 ml). Concentrated the organic layer under reduced pressure maintaining temperature below 45°C to get the residual mass. Charged methanol (1000 ml), heated to reflux and maintained for 3 hours. Cooled the reaction mass to 25°C - 30°C, filtered the solid and dried till constant weight to get (2-chloro-5 -iodophenyl)(4-ethoxyphenyl)methanone.Yield = 201 gm (73.47percent). |
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