HRID878916

反应详情

EQUATION

反应方程式

HRID 878916 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.5 g (30 mmol) of butyl ethylphosphonite (produced as in Example 2) are dissolved in 30 ml of toluene and at 0° C. admixed with 0.72 g (30 mmol) of sodium hydride. After stirring for one hour 5.68 g (40 mmol) of boron trifluoride etherate are added and ethylene oxide is passed in followed by further reaction for two hours. Then, aqueous ammonium chloride solution is added followed by warming to room temperature. This is followed by concentrating in vacuo, taking up in diethyl ether, removal of insoluble salts by filtration and renewed concentrating. Chromatographic purification leaves 4.5 g (78% of theory) of butyl ethyl(2-hydroxyethyl)phosphinate as oil.

WORKUP

后处理

  1. additionare added
  2. customin followed by further reaction for two hours
  3. concentrationby concentrating in vacuo
  4. customremoval of insoluble salts
  5. filtrationby filtration
  6. concentrationrenewed concentrating
  7. customChromatographic purification