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

HRID 2274013ノート

反応式

HRID 2274013 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-01fbd53a8616444ba4e080893ec11ecc
出典データセット
uspto-grants-2015_09
特許番号
US09126945B2

反応ノート

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