HRID1977285
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
To a solution of 1-bromo-4-(7-bromoheptylthio)benzene (5 g) in methanol (25 ml) was added 28% sodium mehtylate in nethanol (7.9 g) and the mixture was stirred under refluxing for 2 hours. The residue was adjusted to pH 2 with dilute HCl aq. and extracted with ethyl acetate. The organic layer was seperated, wahsed with brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (50:1) to give 1-bromo-4-(7-methoxyheptylthio)benzene (3.59 g).
WORKUP
后处理
- temperatureunder refluxing for 2 hours
- extractionextracted with ethyl acetate
- customThe organic layer was seperated
- dry with materialdried over magnesium sulfate
- customevaporated under reduced pressure
- customThe residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (50:1)