HRID1612665

反应详情

EQUATION

反应方程式

HRID 1612665 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.0 g of ethyl 3-amino-2-(p-chlorophenyl)propyl(diethoxymethyl)phosphinate in 5 ml of methanol are added 2.5 ml of a 2 normal sodium hydroxide solution and the mixture is heated to a temperature of 80° for a period of 5 hours. After this time, the reaction is concentrated under reduced pressure, and the oily residue is passed down an Ion Exchange Resin (DOWEX® 50W-X8 H+) using de-ionised water as eluant. Ninhydrin-positive fractions are combined and evaporated to give 3-amino-2-(4-chlorophenyl)-propyl(diethoxymethyl)phosphinic acid, m.p. 175°-185° (dec.), 31P-NMR: δ=+31.6 ppm (D2O).

WORKUP

后处理

  1. temperaturethe mixture is heated to a temperature of 80° for a period of 5 hours
  2. concentrationAfter this time, the reaction is concentrated under reduced pressure
  3. customevaporated