反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- customis removed in vacuo
- customto afford a pale yellow oil
- stirringthe clear pale yellow solution is stirred overnight at room temperature
- customThe solvent is removed in vacuo