HRID2106648

反应详情

EQUATION

反应方程式

HRID 2106648 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

168.3 g (1.22 mol) of potassium carbonate are added to a solution of 61.6 g (406 mmol) of 4-piperidinemethanol hydrochloride in a mixture of 406 ml of chloroform and 406 ml of water, followed by 42.55 ml (440 mmol) of ethyl chloroformate dissolved in 160 ml of chloroform. The mixture is stirred for 3 h at 20° C., the organic phase is separated off, the aqueous phase is extracted with dichloromethane, the organic phases are combined to form a single phase, washed with water and dried over magnesium sulphate, and the solvents are evaporated off under reduced pressure. 76 g of an oil is obtained, this being used without further treatment in the following stage.

WORKUP

后处理

  1. customthe organic phase is separated off
  2. extractionthe aqueous phase is extracted with dichloromethane
  3. customto form a single phase
  4. washwashed with water
  5. dry with materialdried over magnesium sulphate
  6. customthe solvents are evaporated off under reduced pressure