反应详情

To a mixture of 2.2 g 1-carbobenzyloxy-4-hydroxy-4-anilinomethylpiperidine, 3 ml triethylamine and 20 ml dichloromethane is added a solution of 3 g phosgene in 25 ml toluene. After 30 minutes the mixture is washed with 100 ml, 1 N hydrochloric acid. Removal of solvent by evaporation followed by recrystallization from diethyl ether-hexane affords 1.2 g of 3-phenyl-8-carbobenzyloxy-1-oxa-3,8-diazaspiro[4.5]decan-2-one, mp 100°-102°.

1. washAfter 30 minutes the mixture is washed with 100 ml, 1 N hydrochloric acid
2. customRemoval of solvent
3. customby evaporation
4. customfollowed by recrystallization from diethyl ether-hexane