p-Toluenesulfonic acid → HCID 20367191, 화합물

HRID 460915노트

반응식

HRID 460915 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 20367191HCID 20367191, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-9b1d9579ab3e447cb156ef503ffadca8
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061653

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