HRID28086

反应详情

EQUATION

反应方程式

HRID 28086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 7.1 g of 1-methylethyl 2.2-dichloro-2[(1-methylethoxy)phenylphosphinyl]acetate in 150 ml of ether was added 14 ml of a solution of 1.6 M n-butyl lithium in hexane at -70° over 15 minutes. The solution was then allowed to warm to -10° before adding 60 ml of 0.5 M aqueous HCl solution at -10° to 0°. The phases were separated and the organic phase washed with water then 5% NaHCO3 solution. The solution was then dried and stripped to give 5.0 g of 1-methylethyl 2-chloro-2[(1-methylethoxy)phenylphosphinyl]acetate as a light yellow oil ND25 1.5057.

WORKUP

后处理

  1. temperatureto warm to -10°
  2. customThe phases were separated
  3. washthe organic phase washed with water
  4. customThe solution was then dried