Water → 3-Chloro-5-(trifluoromethyl)pyridine-2-carboxylic acid

HRID 1532561

反応式

HRID 1532561 の反応式
[Cl:1][C:2]1[C:3]([C:12]([O:14]CC)=[O:13])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.O.[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[C:3]([C:12]([OH:14])=[O:13])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:9])[F:10])[CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 22013558Ethyl 3-chloro-5-(trifluoromethyl)pyridine-2-carboxylate

生成物 1

HCID 28219083-Chloro-5-(trifluoromethyl)pyridine-2-carboxylic acid収率 84.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

423 g of ethyl 3-chloro-5-trifluoromethyl-2-pyridinecarboxylate (Example H2) is initially introduced into a mixture of 800 ml of water and 160 ml of ethanol. 800 ml of a 2N sodium hydroxide solution are added dropwise at a temperature below 35° C. After 3 hours, the mixture is washed twice with methylene chloride and then rendered acid with an excess of concentrated hydrochloric acid, while cooling in an ice-bath. The slurry formed is filtered and the solid is washed with water and dried in vacuo. 318 g of the desired product are obtained as a white solid of melting point 135° C. (decomposition).

後処理

  1. washthe mixture is washed twice with methylene chloride
  2. temperaturewhile cooling in an ice-bath
  3. customThe slurry formed
  4. filtrationis filtered
  5. washthe solid is washed with water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-f64f025ff8dd4437abebd97f4a7fdd47
出典データセット
uspto-grants-2001_03
特許番号
US06204221B1

関連ノート

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