HRID991261

反应详情

EQUATION

反应方程式

HRID 991261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

450.3 g of 1,2-dichloroethane (4.55 mol), 15.5 g of polyethylene glycol dimethyl ether (mean molar mass 250 g/mol) and 168.0 g of potassium carbonate (1.2 mol) were initially introduced, and the reaction mixture was heated until the 1,2-dichloroethane refluxes. 118.9 g of dimethyl malonate (0.9 mol) and 1.25 g of tetrabutylammonium bromide (3.88 mmol) were then added at the boil. The mixture was stirred using a finely dispersing stirrer (Ultra Turrax) for 6 hours. Water formed during the reaction was removed by azeotropic distillation with 1,2-dichloroethane throughout the reaction. Further work-up was carried out analogously to Comparative Example 2. The yield was 96.3%.

WORKUP

后处理

  1. additiona finely dispersing stirrer (Ultra Turrax) for 6 hours
  2. customwas removed by azeotropic distillation with 1,2-dichloroethane throughout the reaction