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

HRID 1249438노트

반응식

HRID 1249438 반응식
[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]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 13654087HCID 13654087, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-8a2980e4bc7c4469a8630219f13e797b
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04631343

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