HRID1526926

反应详情

EQUATION

反应方程式

HRID 1526926 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 (prepared 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 one hour of stirring, 5.68 g (40 mmol) of boron trifluoride etherate are added and ethylene oxide is passed in and the mixture is subsequently reacted for a further two hours. Thereafter, aqueous ammonium chloride solution is added and the mixture is warmed to room temperature. That is subsequently concentrated in vacuo, the residue is taken up in diethyl ether, insoluble salts are filtered off and the mixture is again concentrated. Chromatographic purification leaves 4.5 g (78% of theory) of butyl ethyl(2-hydroxyethyl)phosphinate being obtained as oil.

WORKUP

后处理

  1. customis subsequently reacted for a further two hours
  2. concentrationThat is subsequently concentrated in vacuo
  3. filtrationinsoluble salts are filtered off
  4. concentrationthe mixture is again concentrated
  5. customChromatographic purification