2-Propenoic acid, 2-cyano-3-ethoxy-, ethyl ester → HCID 13654083、化合物

HRID 280450ノート

反応式

HRID 280450 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:8]=[C:7]([Cl:9])[CH:6]=[CH:5][C:4]=1[NH:10][NH2:11].[CH2:14]([O:16][C:17](=[O:25])[C:18](=[CH:21]OCC)[C:19]#[N:20])[CH3:15]>C(O)(=O)C.O>[NH2:20][C:19]1[N:10]([C:4]2[CH:5]=[CH:6][C:7]([Cl:9])=[CH:8][C:3]=2[C:2]([F:1])([F:12])[F:13])[N:11]=[CH:21][C:18]=1[C:17]([O:16][CH2:14][CH3:15])=[O:25]

参加物

5

反応物 2

HCID 789432-Propenoic acid, 2-cyano-3-ethoxy-, ethyl esterHCID 2778240(4-Chloro-2-(trifluoromethyl)phenyl)hydrazine

生成物 1

HCID 13654083HCID 13654083、化合物収率 85.9%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

A solution of 31.58 g of 2-(trifluoromethyl)-4-chlorophenylhydrazine and 27.92 g of ethyl(ethoxymethylene)cyanoacetate dissolved in 225 of acetic acid and 75 ml of water was heated on a steam bath for approximately 16 hours. The reaction mixture was cooled to room temperature and placed in the refrigerator. The precipitated solid was collected by filtration and combined with the solids isolated from the filtrate to provide 43 g of 5-amino-1-[2-(trifluoromethyl)-4-chlorophenyl]-1H-pyrazole-4-carboxylic acid, ethyl ester. MP=114°-116° C.

後処理

  1. temperaturewas heated on a steam bath for approximately 16 hours
  2. filtrationThe precipitated solid was collected by filtration
  3. customisolated from the filtrate

出典と根拠

ORDレコード
ord-9726254e7b62442ab15a5e8aa42de1e7
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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