HRID476778

反应详情

EQUATION

反应方程式

HRID 476778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

40 g H2O2 (0.35 mol, 30% solution) was added dropwise while cooling with water and with intense agitation to 80 g (0.25 mol) sec.-butyl-di-n-octyl phosphine in a 500 ml-double-walled vessel. After all had been added, the reaction solution was heated to 70° C. over a period of 30 minutes, while stirring was interrupted. An aqueous phase which deposited on the bottom of the vessel was separated. It was admixed with 4.5 ml sodium carbonate solution (30 g/l) and the pH increased from 5.6 to 9.2. The whole was stirred over a period of 1 hour at 80° C. and allowed to deposit. The aqueous phase was separated and the crude product was distilled in vacuum.

WORKUP

后处理

  1. additionAfter all had been added
  2. customwas separated
  3. temperaturethe pH increased from 5.6 to 9.2
  4. stirringThe whole was stirred over a period of 1 hour at 80° C.
  5. customThe aqueous phase was separated
  6. distillationthe crude product was distilled in vacuum