HRID1073339

反应详情

EQUATION

反应方程式

HRID 1073339 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

The same apparatus as used in Example 1 was employed. To the flask were continuously fed 1,075 g of 30% aqueous sodium hydroxide solution and 1,500 g of a cyclohexane solution which had been prepared by dissolving, in 750 g of cyclohexane, 750 g of di-n-butyltin dibromide containing 1.8% tri-n-butyltin bromide and 1.5% mono-n-butyltin tribromide. The above feeding was performed with stirring and heating at 70° C., to conduct hydrolysis for 45 minutes. To the resulting reaction mixture overflowed was added 3,600 g of water, and the mixture was then allowed to stand, whereby it split into three distinct phases. The specific gravities of the upper, intermediate and lower phases were 0.6, 1.1 and 1.3 respectively. The lower phase was separated out, washed with water, and then dried under reduced pressure, thereby obtaining 445 g of a white substance of di-n-butyltin oxide. Acid titration revealed that its purity was 99.8%, and the oxide had an average particle diameter of 50 μm.

WORKUP

后处理

  1. customhad been prepared
  2. customhydrolysis for 45 minutes
  3. customTo the resulting reaction mixture
  4. customwhereby it split into three distinct phases
  5. customThe lower phase was separated out
  6. washwashed with water
  7. customdried under reduced pressure