HRID1612763

反应详情

EQUATION

反应方程式

HRID 1612763 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 0.642 g of ethyl 3-(N-tert.-butoxycarbonylamino)-2-oxo-propyl(n-butyl)phosphinate in 10 ml of anhydrous dichloromethane under an inert atmosphere is treated with 1.53 g of trimethylbromosilane. After stirring for 7 hours at room temperature the volatile material is removed in vacuo to afford a pale yellow oil. This oil is dissolved in methanol containing 1% of water, and the clear pale yellow solution is stirred overnight at room temperature. The solvent is removed in vacuo to afford 3-amino-2-oxo-propyl(n-butyl)phosphinic acid hydrobromide, m.p. 135°-138°. Suspension in ethanol and treatment with propylene oxide affords 3-amino-2-oxo-propyl(n-butyl)phosphinic acid of m.p. 128°-130°.

WORKUP

后处理

  1. customis removed in vacuo
  2. customto afford a pale yellow oil
  3. stirringthe clear pale yellow solution is stirred overnight at room temperature
  4. customThe solvent is removed in vacuo