HRID1027224
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 5 L round bottom flask fitted with an overhead stirrer, thermocouple and N2 inlet, was added 4-bromo-3-methoxyphenol (254 g, 1251 mmol), DCM (2500 mL) and DIPEA (437 mL, 2502 mmol). The reaction mixture was cooled in an ice bath, followed by addition of tert-butylchlorodimethylsilane (198 g, 1314 mmol). The reaction mixture was stirred at RT overnight, and then diluted with water. The organic layer was separated, dried over sodium sulfate, filtered and concentrated to provide (4-bromo-3-methoxyphenoxy)(tert-butyl)dimethylsilane (472 g, 1250 mmol, 100% yield). MS (M+1)=319.2.
WORKUP
后处理
- customTo a 5 L round bottom flask fitted with an overhead stirrer
- temperatureThe reaction mixture was cooled in an ice bath
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated