HRID280977

反应详情

EQUATION

反应方程式

HRID 280977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-(1-benzyloxycarbonyl-4-piperidyl)valeric acid (54.8 g), sodium bicarbonate (29 g), ethyl iodide (21 ml) and N,N-dimethylformamide (150 ml) is stirred for 3 hours at 70°-80° C. After further addition of ethyl iodide (10 ml), the stirring is continued for further 3 hours at 90°-100° C. After cooling, the mixture is diluted with water and extracted with ethyl acetate (1 l). The extract is washed successively with water, 1N hydrochloric acid and sodium bicarbonate solution, dried over anhydrous magnesium sulfate and evaporated in vacuo to yield ethyl 5-(1-benzyloxycarbonyl-4-piperidyl)valerate (58 g) as a pale yellow oil.

WORKUP

后处理

  1. waitthe stirring is continued for further 3 hours at 90°-100° C
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate (1 l)
  4. washThe extract is washed successively with water, 1N hydrochloric acid and sodium bicarbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated in vacuo