Methylamine → 1-[4-Chloro-2-(trifluoromethyl)phenyl]-5-cyano-N-methyl-1H-pyrazole-4-carboxamide

HRID 280452ノート

反応式

HRID 280452 の反応式
[C:1]([C:3]1[N:7]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=2[C:15]([F:18])([F:17])[F:16])[N:6]=[CH:5][C:4]=1[C:19]([O:21]CC)=O)#[N:2].[CH3:24][NH2:25]>CN(C=O)C>[C:1]([C:3]1[N:7]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=2[C:15]([F:17])([F:18])[F:16])[N:6]=[CH:5][C:4]=1[C:19]([NH:25][CH3:24])=[O:21])#[N:2]

参加物

4

反応物 2

HCID 6329MethylamineHCID 13654087HCID 13654087、化合物

生成物 1

HCID 136540901-[4-Chloro-2-(trifluoromethyl)phenyl]-5-cyano-N-methyl-1H-pyrazole-4-carboxamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 1.23 g of 5-cyano-1-[2-(trifluoromethyl)-4-chlorophenyl]-1H-pyrazole-4-carboxylic acid, ethyl ester and 8 ml of 40% aqueous monomethylamine in 20 ml of DMF was stirred at approximately 25° C. for 16 hours. The reaction mixture was poured into 150 ml of ice water and the precipitated solid was collected by filtration. The isolated material was recrystallized from ethanol to provide 535 mg of 5-cyano-1-[2-(trifluoromethyl)-4-chlorophenyl]-N-methyl-1H-pyrazole-4-carboxamide. MP=162.5°-164° C.

後処理

  1. filtrationthe precipitated solid was collected by filtration
  2. customThe isolated material was recrystallized from ethanol

出典と根拠

ORDレコード
ord-02e51c81fbe3429e96ebc84c73f968a2
出典データセット
uspto-grants-1986_05
特許番号
US04589905

反応ノート

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