2-Methylbenzenesulfonic acid → 3-Amino-1-(3-chloro-4-bromobenzyl)-pyrazol-5-one

HRID 460893

反応式

HRID 460893 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([CH2:6][NH:7][NH2:8])=[CH:4][C:3]=1[Cl:11].C([O:14][C:15](=O)[CH:16]=[C:17]([NH2:21])OCC)C.C1(C)C(S(O)(=O)=O)=CC=CC=1>C(O)C>[NH2:21][C:17]1[NH:8][N:7]([CH2:6][C:5]2[CH:9]=[CH:10][C:2]([Br:1])=[C:3]([Cl:11])[CH:4]=2)[C:15](=[O:14])[CH:16]=1

参加物

5

反応物 3

HCID 69252-Methylbenzenesulfonic acidHCID 278451beta-Aminobeta-ethoxyacrylic acid ethyl esterHCID 20495799[(4-Bromo-3-chlorophenyl)methyl]hydrazine

生成物 1

HCID 203672203-Amino-1-(3-chloro-4-bromobenzyl)-pyrazol-5-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

48.8 g of 4-bromo-3-chlorobenzylhydrazine are added dropwise under nitrogen to a solution of 33.2 g of β-amino-β-ethoxyacrylic acid ethyl ester and 1.5 g of toluenesulphonic acid in 150 ml of ethanol. After stirring for a further two hours, the mixture was left to stand and the compound identified above began to crystallise out after four hours. It was filtered off and twice recrystallised from ethanol. Melting point: 145°-146°, 23 g (37%).

後処理

  1. waitthe mixture was left
  2. customto crystallise out after four hours
  3. filtrationIt was filtered off
  4. customtwice recrystallised from ethanol

出典と根拠

ORDレコード
ord-b1355b9f8c884251b2a602436be410aa
出典データセット
uspto-grants-1977_12
特許番号
US04061653

関連ノート

読み込み中…