HRID865845
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 0.5 g of isobutyl P-(3-tert.-butoxycarbonylamino-2-oxo-propyl)-P-methyl-phosphinate in 10 ml of 36% aqueous hydrochloric acid is heated to reflux for a period of 4 hours. The mixture is then allowed to cool to room temperature, concentrated under reduced pressure, and coevaporated twice with 20 ml of water. The crude product is dissolved in 20 ml of ethanol, 1 ml of propylene oxide is added, and the mixture is stirred until the precipitated solid is free of halogen. The solid is filtered and dried to give P-(3-amino-2-oxo-propyl)-P-methyl-phosphinic acid, m.p. 148°-149°, 31P-NMR spectrum: δ=32.8 ppm (D2O).
WORKUP
后处理
- temperatureto reflux for a period of 4 hours
- concentrationconcentrated under reduced pressure
- dissolutionThe crude product is dissolved in 20 ml of ethanol
- addition1 ml of propylene oxide is added
- filtrationThe solid is filtered
- customdried