Reaktion #569813

Reaktionsgleichung

methyl chloroformate

N-(4-trifluoromethylphenyl)-3-(4-propoxyphenyl)-4-(N-propylamino)-4,5,-dihydro-1H-pyrazole-1-carboxamide

pyridine

→

desired compound

Ausbeute 41.9%

N-(4-trifluoromethylphenyl)-3-(4-propoxyphenyl)-4-(N-methoxycarbonyl-N-propylamino)-4,5,-dihydro-1H-pyrazole-1-carboxamide

Ausbeute 41.9%

Lösungsmittel

ethyl acetate

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenthe reaction mixture was washed with water and brine
2. 2
   Einengenconcentrated in vacuo
3. 3
   Sonstigechromatographed over silica gel

Vorschrift

To 1.5 g (3.3 mmole) of N-(4-trifluoromethylphenyl)-3-(4-propoxyphenyl)-4-(N-propylamino)-4,5,-dihydro-1H-pyrazole-1-carboxamide Example (586) dissolved in 25 ml of ethyl acetate and cooled to -5° C., was added 1.2 g (15 mmole) of pyridine and, finally, 1.3 g (13 mmole) of methyl chloroformate in 10 ml of ethyl acetate was added over 30 minutes. After an additional 30 minutes, the reaction mixture was washed with water and brine, concentrated in vacuo, and chromatographed over silica gel using hexanes and ethyl acetate to yield 0.7 g of the desired compound, mp 142°-145° C.

Quelle