HRID1816686
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
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
A mixture of 1-bromo-4-(6-bromohexyloxy)benzene (6.0 g) and sodium methylate (28% in methanol) (10.3 ml) in methanol (30 ml) was stirred for 2 hours at 70° C. (bath temp.), and then the solvent was evaporated. The residue was neutralized by 1N-hydrochloric acid and extracted with ethyl acetate (100 ml), and washed with water and brine. The organic layer was dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure to give a crude product. The crude product was purified by silica gel chromatography (20:1-10:1 hexane-ethyl acetate) to give 1-bromo-4-(6-methoxyhexyloxy)benzene (15.61 g) as a colorless oil.
WORKUP
后处理
- customthe solvent was evaporated
- extractionextracted with ethyl acetate (100 ml)
- washwashed with water and brine
- dry with materialThe organic layer was dried over magnesium sulfate
- filtrationMagnesium sulfate was filtered off
- customthe filtrate was evaporated under reduced pressure
- customto give a crude product
- customThe crude product was purified by silica gel chromatography (20:1-10:1 hexane-ethyl acetate)