反应详情

Sodium hydride (0.090 g, 60% dispersion in mineral oil) was added to a solution of 4-trifluoromethyl-3-pyridinecarboxamide (0.40 g) in N,N-dimethylformamide at 20° C., and stirred for 1 hour. Benzyl isocyanate (0.31 ml) was added and the mixture stirred at 20° C. for 2 hours, then methyl bromoacetate (0.30 ml) added and stirring continued for 5 hours. Ethyl acetate and water were added to the solution and the organic phase dried (magnesium sulfate), evaporated and the residue purified by column chromatography on silica gel, eluting with n-hexane/ethyl acetate (2:1), to give 3-benzyl-1-(4-trifluoromethyl-3-pyridylcarbonyl)hydantoin (0.50 g, Compound S-132).

1. stirringthe mixture stirred at 20° C. for 2 hours
2. stirringstirring
3. waitcontinued for 5 hours
4. dry with materialthe organic phase dried (magnesium sulfate)
5. customevaporated
6. customthe residue purified by column chromatography on silica gel
7. washeluting with n-hexane/ethyl acetate (2:1)