HRID347618

反应详情

EQUATION

反应方程式

HRID 347618 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

100 g (0.63 mol) of (±)-1-phenyl-1,2-ethanediol (3) (87% pure according to GC) according to Example 1, 200 ml of toluene, 32 g (0.24 mol) of paraldehyde and 1 g of para-toluenesulfonic acid were charged to a 1 l stirrer, heated to boiling (110° C.) and stirred under reflux for a period of 4 h. A total of 10 ml of water were eliminated. After this time, the mixture was cooled to 20° C. and washed until neutral with sodium carbonate solution and water, and the solvent was distilled off under reduced pressure, leaving 103 g of crude product (85.3% pure according to GC). GC conditions see Example 2.

WORKUP

后处理

  1. additionwere charged to a 1 l stirrer
  2. temperatureheated
  3. custom(110° C.)
  4. temperatureunder reflux for a period of 4 h
  5. washwashed until neutral with sodium carbonate solution and water
  6. distillationthe solvent was distilled off under reduced pressure