HRID1198461

反应详情

EQUATION

反应方程式

HRID 1198461 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1.3 g of ethyl 1-(2,2-dimethyl-1-oxopropyl)-4-oxo-3-piperidinecarboxylate and 0.75 g of valeramidine hydrochloride in 10 ml of anhydrous ethyl alcohol is treated with 5.3 ml of a 1M solution of sodium methoxide in methanol. The resulting mixture is stirred and heated at reflux for one hour. The reaction mixture is allowed to cool over 30 minutes then filtered. The filtrate is evaporated to a gummy residue and stirred with 40 ml of ether for 30 minutes, filtered and the cake washed with ether. The cake is dried at 56° C. under vacuum to afford 1.0 g of the desired product as a colorless solid, m.p. 167°-172° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for one hour
  3. temperatureto cool over 30 minutes
  4. filtrationthen filtered
  5. customThe filtrate is evaporated to a gummy residue
  6. stirringstirred with 40 ml of ether for 30 minutes
  7. filtrationfiltered
  8. washthe cake washed with ether
  9. customThe cake is dried at 56° C. under vacuum