반응 #48554

반응 방정식

4-chlorophenyl isothiocyanate

ethyl 4-methylpiperidine-4-carboxylate

→

title compound

Ethyl 1-{[(4-chlorophenyl)amino]carbonothioyl}-4-methylpiperidine-4-carboxylate

용매

dichloromethane

반응 조건

후처리

1. 1
   기타The mixture was partitioned between dichloromethane and brine
2. 2
   기타the layers were separated
3. 3
   건조The organic phase was dried over MgSO4
4. 4
   기타evaporated under reduced pressure
5. 5
   기타The crude product was purified by column chromatography on silica gel

실험 절차

A mixture of 4-chlorophenyl isothiocyanate (2.36 g, 13.98 mmol), and ethyl 4-methylpiperidine-4-carboxylate (U.S. 2002/0086887, example 532C) (2.17 g, 12.71 mmol) in dichloromethane (50 mL) was stirred at room temperature for 30 minutes. The mixture was partitioned between dichloromethane and brine, and the layers were separated. The organic phase was dried over MgSO4 and evaporated under reduced pressure. The crude product was purified by column chromatography on silica gel using dichloromethane:ethyl acetate (100:0 to 90:10) to provide the title compound as a white solid, 3.46 g.

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