HRID1600874

反应详情

EQUATION

反应方程式

HRID 1600874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

At 20° C., a solution of 15 g (60 mmol) of methyl 2-[2-(tetrahydropyran-2-yloxy)phenyl]-acrylate in 36 ml of methyl formate is added dropwise to a suspension of 1.96 g (66 mmol) of sodium hydride (80% strength) in 50 ml of dimethylformamide. After 4 hours, 15 g of potassium carbonate and 9 g of chloroacetonitrile are added to this mixture, which is stirred at 20° C. for a further 14 hours and then poured into water. The reaction mixture is extracted with ethyl acetate and the organic phase is dried over sodium sulphate and concentrated under reduced pressure. 15.9 g (83.55% of theory) of methyl 2-[2-(tetrahydropyran-2-yloxy)-phenyl]-3-cyanomethoxy-acrylate are obtained.

WORKUP

后处理

  1. extractionThe reaction mixture is extracted with ethyl acetate
  2. dry with materialthe organic phase is dried over sodium sulphate
  3. concentrationconcentrated under reduced pressure