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Sodium Hydroxide → 5-amino-1-methyl-3-(trifluoromethyl)-1H-Pyrazole-4-carboxylic acid

HRID 1978167
ノート
印刷プレビュー

反応式

HRID 1978167 の反応式
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([F:11])([F:10])[F:9])[C:3]=1[C:12]([O:14]CC)=[O:13].[OH-].[Na+]>O>[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([F:11])([F:10])[F:9])[C:3]=1[C:12]([OH:14])=[O:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 98376025-Amino-1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester

生成物 1

HCID 101305025-amino-1-methyl-3-(trifluoromethyl)-1H-Pyrazole-4-carboxylic acid収率 85.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

To 10 ml of water, 2.37 g (10 mmol) of ethyl 5-amino-1-methyl-3-trifluoromethylpyrazole-4-carboxylate and 0.44 g (11 mmol) of sodium hydroxide were added and stirred at 60° C. for 10 hours. After cooling to room temperature, the reaction mixture was washed with toluene. The resulting aqueous solution was made pH 1 by adding concentrated hydrochloric acid. Precipitate was filtered and dried to obtain 1.78 g of desired 5-amino-1-methyl-3-trifluoromethylpyrazole-4-carboxylic acid as white solid. The yield was 85% Following results were obtained by NMR analysis.

後処理

  1. temperatureAfter cooling to room temperature
  2. washthe reaction mixture was washed with toluene
  3. additionby adding concentrated hydrochloric acid
  4. filtrationPrecipitate was filtered
  5. customdried

出典と根拠

ORDレコード
ord-f8f3dbff06d54d1c8943fb2727e273d8
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06235911B1

反応ノート

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