Methylamine → 1-[4-Chloro-2-(trifluoromethyl)phenyl]-5-cyano-N-methyl-1H-pyrazole-4-carboxamide

HRID 1249438Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1249438
[C:1]([C:3]1[N:7]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=2[C:15]([F:18])([F:17])[F:16])[N:6]=[CH:5][C:4]=1[C:19]([O:21]CC)=O)#[N:2].[CH3:24][NH2:25]>CN(C=O)C>[C:1]([C:3]1[N:7]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=2[C:15]([F:17])([F:18])[F:16])[N:6]=[CH:5][C:4]=1[C:19]([NH:25][CH3:24])=[O:21])#[N:2]

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 13654087HCID 13654087, Verbindung

Produkt 1

HCID 136540901-[4-Chloro-2-(trifluoromethyl)phenyl]-5-cyano-N-methyl-1H-pyrazole-4-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 1.23 g of 5-cyano-1-[2-(trifluoromethyl)-4-chlorophenyl]-1H-pyrazole-4-carboxylic acid, ethyl ester and 8 ml of 40% aqueous monomethylamine in 20 ml of DMF was stirred at approximately 25° C. for 16 hours. The reaction mixture was poured into 150 ml of ice water and the precipitated solid was collected by filtration. The isolated material was recrystallized from ethanol to provide 535 mg of 5-cyano-1-[2-(trifluoromethyl)-4-chlorophenyl]-N-methyl-1H-pyrazole-4-carboxamide. mp=162.5°-164° C.

Aufarbeitung

  1. filtrationthe precipitated solid was collected by filtration
  2. customThe isolated material was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-8a2980e4bc7c4469a8630219f13e797b
Quelldatensatz
uspto-grants-1986_12
Patentnummer
US04631343

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