HRID434776

反应详情

EQUATION

反应方程式

HRID 434776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of sodium ethoxide in toluene (50 ml) was prepared as in (a) above and to this was added diethyl oxalate (10.9 g) and a solution of ethyl 3-(hydroxymethylphosphinyl)propanoate (13.5 g) in toluene (75 ml). The mixture was stirred for 16 hours then extracted with water (4×60 ml). The extract was acidified with conc. hydrochloric acid (200 ml) and the acid solution refluxed for 2.5 hours. The crude product (8.8 g) was isolated as in part (a) and triturated with acetone to give the desired product (5.2 g).

WORKUP

后处理

  1. extractionthen extracted with water (4×60 ml)
  2. temperaturethe acid solution refluxed for 2.5 hours
  3. customThe crude product (8.8 g) was isolated as in part (a)
  4. customtriturated with acetone