Hydrochloric Acid → 2-Chloro-5-({[1-methyl-3-(pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazol-5-yl]carbonyl}amino)benzoic acid

HRID 2274013노트

반응식

HRID 2274013 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([NH:12][C:13]([C:15]2[N:19]([CH3:20])[N:18]=[C:17]([C:21]([F:27])([F:26])[C:22]([F:25])([F:24])[F:23])[C:16]=2[C:28]([F:31])([F:30])[F:29])=[O:14])=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].[OH-].[Na+].Cl>CO>[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([NH:12][C:13]([C:15]2[N:19]([CH3:20])[N:18]=[C:17]([C:21]([F:27])([F:26])[C:22]([F:25])([F:23])[F:24])[C:16]=2[C:28]([F:29])([F:30])[F:31])=[O:14])=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86660079methyl 2-chloro-5-({[1-methyl-3-(pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazol-5-yl]carbonyl}amino)benzoate

생성물 1

HCID 462196652-Chloro-5-({[1-methyl-3-(pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazol-5-yl]carbonyl}amino)benzoic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

5.75 g (11.9 mmol) of methyl 2-chloro-5-({[1-methyl-3-(pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazol-5-yl]carbonyl}amino)benzoate are dissolved in 30 ml of methanol p.A., and 15.0 ml (30.0 mmol) of 2 N aqueous sodium hydroxide solution are then added. The reaction mixture is stirred at room temperature for 16 hours. The reaction solution is acidified carefully with 6 N hydrochloric acid, and the aqueous phase is then extracted three times with ethyl acetate. The combined organic phases are washed once with saturated sodium chloride solution, dried over sodium sulphate and filtered. The solvent is removed under reduced pressure on a rotary evaporator. This gives 5.57 g of 2-chloro-5-({[1-methyl-3-(pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazol-5-yl]carbonyl}amino)benzenecarboxylic acid as a colourless solid.

후처리

  1. extractionthe aqueous phase is then extracted three times with ethyl acetate
  2. washThe combined organic phases are washed once with saturated sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. customThe solvent is removed under reduced pressure on a rotary evaporator

출처 및 근거

ORD 기록
ord-01fbd53a8616444ba4e080893ec11ecc
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126945B2

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