HRID1603207

反应详情

EQUATION

反应方程式

HRID 1603207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

In a 750 ml sulfonating flask with mechanical stirrer, condenser and 100 ml dropping funnel 64.0 g (1.6 mol) of sodium hydroxide are dissolved in 64 ml of water under an argon atmosphere. 170 ml of toluene, 10.3 g (31.8 mmol) of tetrabutylammonium bromide and 50 g (318 mmol) of 4-hydroxy-2,2,6,6-tetramethylpiperidine are added. 58.8 g (636 mmol) of epichlorohydrin are added dropwise at 45° C. The mixture is then stirred at 50° C. for 4 hours. The reaction mixture is cooled to room temperature and then poured into 1 l of ice-water, the organic phase is separated off and dried over sodium sulfate, and the residue is concentrated on a rotatory evaporator. The residue is distilled at 8·10-3 torr. Boiling point: 48° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. customthe organic phase is separated off
  3. dry with materialdried over sodium sulfate
  4. concentrationthe residue is concentrated on a rotatory evaporator
  5. distillationThe residue is distilled at 8·10-3 torr