HRID553296
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated
- temperatureto reflux for 75 minutes
- temperatureOn cooling the reaction mixture
- extractionextracted with ethyl acetate
- customThe organic phase was separated
- washwashed sequentially with 2M aqueous hydrochloric acid (2×50 mL), brine (50 mL)
- dry with materialdried (magnesium sulfate)
- concentrationconcentrated
- customPurification on silica
- washeluting iso-hexane/ethyl acetate [4:1 to 1:1 to 0:1]