Sodium Cyanide → HCID 13654087, 화합물

HRID 280451노트

반응식

HRID 280451 반응식
Cl[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=2[C:14]([F:17])([F:16])[F:15])[N:5]=[CH:4][C:3]=1[C:18]([O:20][CH2:21][CH3:22])=[O:19].[C-:23]#[N:24].[Na+]>CN(C)C=O>[C:23]([C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=2[C:14]([F:17])([F:16])[F:15])[N:5]=[CH:4][C:3]=1[C:18]([O:20][CH2:21][CH3:22])=[O:19])#[N:24]

참가 물질

4

반응물 2

HCID 8929Sodium CyanideHCID 13654085HCID 13654085, 화합물

생성물 1

HCID 13654087HCID 13654087, 화합물수율 32.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 3.15 g of 5-chloro-1-[2-(trifluoromethyl)-4-chlorophenyl]-1H-pyrazole-4-carboxylic acid, ethyl ester and 1.1 g of sodium cyanide in 25 ml of dimethylformamide was heated at approximately 100° C. for four and one-half hours. The reaction mixture also contained approximately 3 g of molecular sieve to insure dryness. The reaction mixture was cooled and poured into approximately 300 ml of ice water. The precipitated solid was collected by filtration and recrystallized from ethanol (charcoal) to provide 1 g of 5-cyano-1-[2-(trifluoromethyl)-4-chlorophenyl]-1H-pyrazole-4-carboxylic acid, ethyl ester. MP=70°-72° C.

후처리

  1. temperatureThe reaction mixture was cooled
  2. filtrationThe precipitated solid was collected by filtration
  3. customrecrystallized from ethanol (charcoal)

출처 및 근거

ORD 기록
ord-34d8f69ec7724bc3a1ee3a54570d3542
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04589905

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