p-Toluenesulfonic acid → HCID 20367191、化合物

HRID 460915ノート

反応式

HRID 460915 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([CH2:6][NH:7][NH2:8])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].C([O:17][C:18](=O)[CH:19]=[C:20]([NH2:24])OCC)C.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)C>[NH2:24][C:20]1[NH:8][N:7]([CH2:6][C:5]2[CH:9]=[CH:10][C:2]([Cl:1])=[C:3]([C:11]([F:12])([F:13])[F:14])[CH:4]=2)[C:18](=[O:17])[CH:19]=1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 278451beta-Aminobeta-ethoxyacrylic acid ethyl esterHCID 23334257(4-Chloro-3-(trifluoromethyl)benzyl)hydrazine

生成物 1

HCID 20367191HCID 20367191、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

67 g of 4-chloro-3-trifluoromethylbenzylhydrazine were added dropwise, under nitrogen, to a solution of 46.1 g of β-amino-β-ethoxyacrylic acid ethyl ester and 2 g of p-toluenesulphonic acid in 250 ml of ethanol. After stirring overnight, the solvent was distilled off in vacuo and the residue, which solidified, was filtered off and recrystallised from ethanol. The product was the compound identified above. Melting point: 132°, 25 g (30%).

後処理

  1. distillationthe solvent was distilled off in vacuo
  2. filtrationwas filtered off
  3. customrecrystallised from ethanol

出典と根拠

ORDレコード
ord-9b1d9579ab3e447cb156ef503ffadca8
出典データセット
uspto-grants-1977_12
特許番号
US04061653

反応ノート

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