HRID973608

反应详情

EQUATION

反应方程式

HRID 973608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 ml of 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

  1. customDuring this time, a white precipitate is formed
  2. customis removed by co-evaporation with 6×50 ml of water on a rotary evaporator
  3. dissolutionThe crude product is then dissolved in 50 ml of ethanol
  4. filtrationFiltration
  5. customdrying