Sodium Cyanide → HCID 13654087、化合物

HRID 1249437ノート

反応式

HRID 1249437 の反応式
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]

参加物

4

反応物 2

HCID 8929Sodium CyanideHCID 13654085HCID 13654085、化合物

生成物 1

HCID 13654087HCID 13654087、化合物収率 32.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-809343cea0b546839bb456aad340b94a
出典データセット
uspto-grants-1986_12
特許番号
US04631343

反応ノート

読み込み中…