Reaktion #569781

Reaktionsgleichung

N-(4-trifluoromethylphenyl)-3-(4-chlorophenyl)-4-carbo-t-butoxyamino-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide

trifluoroacetic acid

→

white solid

Ausbeute 85.0%

N-(4-trifluoromethylphenyl)-3-(4-chlorophenyl)-4-amino-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide

Ausbeute 85.0%

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was refluxed for 40 minutes while gas
2. 2
   Sonstigean additional 20 minutes
3. 3
   EinengenThe mixture was then concentrated in vacuo
4. 4
   Sonstigepartitioned between ethyl ether and dilute aqueous sodium hydroxide
5. 5
   WaschenThe organic layer was washed with brine
6. 6
   Trocknendried over magnesium sulfate
7. 7
   Einengenconcentrated in vacuo
8. 8
   Sonstigethe resulting solid was triturated with hexanes
9. 9
   Filtrationfiltered

Vorschrift

To 74 g (149 mmole) of N-(4-trifluoromethylphenyl)-3-(4-chlorophenyl)-4-carbo-t-butoxyamino-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide (Example 2) was added 74 g of trifluoroacetic acid and 74 g of chloroform. The mixture was refluxed for 40 minutes while gas was evolved and then an additional 20 minutes. The mixture was then concentrated in vacuo and then partitioned between ethyl ether and dilute aqueous sodium hydroxide. The organic layer was washed with brine, dried over magnesium sulfate, concentrated in vacuo, and the resulting solid was triturated with hexanes and filtered yielding 50 g (85%) of a white solid, mp 165°-167° C.

Quelle