HRID553296

反应详情

EQUATION

反应方程式

HRID 553296 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Copper(II) nitrate trihydrate (3.3 g) was added to (3-bromomethyl-4-methoxy-phenyl)-acetic acid (1.4 g) in water (50 mL) and heated to reflux for 75 minutes. On cooling the reaction mixture was acidified with 2M aqueous hydrochloric acid and extracted with ethyl acetate. The organic phase was separated and washed sequentially with 2M aqueous hydrochloric acid (2×50 mL), brine (50 mL), dried (magnesium sulfate) and concentrated. Purification on silica, eluting iso-hexane/ethyl acetate [4:1 to 1:1 to 0:1], to give the subtitle compound as a solid (0.26 g).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 75 minutes
  3. temperatureOn cooling the reaction mixture
  4. extractionextracted with ethyl acetate
  5. customThe organic phase was separated
  6. washwashed sequentially with 2M aqueous hydrochloric acid (2×50 mL), brine (50 mL)
  7. dry with materialdried (magnesium sulfate)
  8. concentrationconcentrated
  9. customPurification on silica
  10. washeluting iso-hexane/ethyl acetate [4:1 to 1:1 to 0:1]