HRID1063342

反应详情

EQUATION

反应方程式

HRID 1063342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl-1-benzyl-4-oxo-piperidine-3-carboxylate hydrochloride (150 g, 0.504 mol) was suspended in a solvent mixture of 750 ml THF and 750 ml DMF at room temperature. Addition of powdered KOH (56 g, 1.0 mol) was made in two equal lots keeping half an hour interval between two additions. To a clear reaction mixture methyl iodide (78 g, 0.55 mol) was added over period of 10 minutes and it was stirred for three hours at room temperature. The reaction was quenched by adding 4 ltr water followed by 1.5 ltr diethyl ether. Layers were separated. Organic layer was washed with water and dried over Na2SO4. Evaporation of organic solvent afforded a liquid, which was passed through a silica gel column to give 86 g (61%), titled compound.

WORKUP

后处理

  1. waitkeeping half an hour
  2. customThe reaction was quenched
  3. additionby adding 4 ltr water
  4. customLayers were separated
  5. washOrganic layer was washed with water
  6. dry with materialdried over Na2SO4
  7. customEvaporation of organic solvent
  8. customafforded a liquid, which