HRID743275
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
2.00 g of 1-t-butoxycarbonyl-4-(2-{2-[2-(3-methoxyphenyl)ethyl]phenoxy}ethyl)piperidine [prepared as described in step (a) above] were dissolved in 10 ml of a 4N solution of hydrogen chloride in dioxane, and the solution was allowed to stand at room temperature for 4 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, and the resulting solid residue was dissolved in a small amount of methylene chloride, after which ethyl acetate was added to the solution. The crystals which precipitated were collected by filtration, to give 1.59 g (yield 93%) of the title compound as colorless crystals, melting at 119°-121° C.
WORKUP
后处理
- customAt the end of this time, the solvent was removed by distillation under reduced pressure
- dissolutionthe resulting solid residue was dissolved in a small amount of methylene chloride
- additionafter which ethyl acetate was added to the solution
- customThe crystals which precipitated
- filtrationwere collected by filtration