HRID1956794
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 refluxing solution of 15.3 g (0.08 mole) (3RS)-1-benzyl-3-hydroxymethyl pyrrolidine in 220 ml CHCl3 was slowly added a solution of 330 ml thionyl chloride in 60 ml CHC13, and the reflux was continued for one hour. The mixture was evaporated and the residue was dissolved in water. The water layer was washed with ethyl acetate and then made alkaline with 0.2M NaOH-solution. The water layer was extracted three times with ethyl acetate and the combined organic layer was dried (Na2SO4), filtered and evaporated to give the product in a quantitative yield (16.8 g)
WORKUP
后处理
- customThe mixture was evaporated
- dissolutionthe residue was dissolved in water
- washThe water layer was washed with ethyl acetate
- extractionThe water layer was extracted three times with ethyl acetate
- dry with materialthe combined organic layer was dried (Na2SO4)
- filtrationfiltered
- customevaporated
- customto give the product in a quantitative yield (16.8 g)