HRID1721855
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 3.89 g of 4-phenyl-4-(4-trifluoromethylphenoxy)piperidine in 25 ml of benzene was added a solution of 0.68 g of methyl isocyanate in 25 ml of benzene. The reaction mixture was stirred for four hours at room temperaure. Evaporation of the volatiles afforded a solid which was purified by means of high pressure liquid chromatography (silica gel; elution with 50% ethyl acetate/dichloromethane). Recrystallization from 30% hexane/isopropyl ether yielded 2.46 g (54.19%) 1-(N-methylamino)carbonyl-4-phenyl-4-(4-trifluoromethylphenoxy)piperidine, m.p. 118°-120° C.
WORKUP
后处理
- customEvaporation of the volatiles
- customafforded a solid which
- customwas purified by means of high pressure liquid chromatography (silica gel; elution with 50% ethyl acetate/dichloromethane)
- customRecrystallization from 30% hexane/isopropyl ether