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

HRID 460893

반응식

HRID 460893 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-b1355b9f8c884251b2a602436be410aa
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061653

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