HRID1374911

反应详情

EQUATION

反应方程式

HRID 1374911 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl 2-(5-bromo-3-pyridyloxy)butyrate (1.37 g) and copper (1) cyanide (0.67 g) in dry N-methylpyrollidin-2-one (5 ml) was stirred at 150° C. under an atmosphere of nitrogen for 3.25 hours then cooled to ambient temperature and stored for 18 hours. The mixture was diluted with water and extracted with ethyl acetate (four times). The extracts were combined, washed with water (three times), dried over magnesium sulphate and evaporated under reduced pressure to give a liquid which was fractionated by chromatography (silica; ethyl acetate) to give the required product, 0.29 g, as an orange oil.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (four times)
  2. washwashed with water (three times)
  3. dry with materialdried over magnesium sulphate
  4. customevaporated under reduced pressure
  5. customto give a liquid which