HRID729135
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 2.4 g of 3-benzyloxycarbonylaminopropyl(dodecyl) phosphinic acid in 50 ml of 36% hydrochloric acid is refluxed for 3 hours. During this time, a white precipitate is formed. After cooling to room temperature the acid is removed by co-evaporation with 6×50 ml of water on a rotary evaporator. The crude product is then dissolved in 50 mlof ethanol and stirred with 5 ml of propylene oxide. Filtration and drying gives 3-aminopropyl(dodecyl) phosphinic acid as a white solid m.p. 175°-7°. 31P-NMR=43.0 ppm. (NaOD).
WORKUP
后处理
- customDuring this time, a white precipitate is formed
- customis removed by co-evaporation with 6×50 ml of water on a rotary evaporator
- dissolutionThe crude product is then dissolved in 50 mlof ethanol
- filtrationFiltration
- customdrying