p-Toluenesulfonic acid → HCID 20367191, Verbindung

HRID 1605731Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1605731
[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

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-4525e44290d2430da1da1d641d8d2233
Quelldatensatz
uspto-grants-1976_04
Patentnummer
US03950528

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