p-Toluenesulfonic acid → HCID 20367191, Verbindung

HRID 460915Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 460915
[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

Komponenten

5

Edukt 3

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

Produkt 1

HCID 20367191HCID 20367191, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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%).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-9b1d9579ab3e447cb156ef503ffadca8
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04061653

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