HRID705432
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 methyl 4-methoxy-2-methylbenzoate (1 g, 5.6 mmol) in CCl4 (25 mL) was added dropwise N-bromosuccinimide (1.1 g, 6.2 mmol) previously dissolved in CCl4 (5 mL) and a catalytic amount of benzoyl peroxide. The mixture was refluxed for 2 hours, cooled to room temperature and poured onto iced water. The aqueous mixture was extracted with DCM (3×), and the combined organics were dried over MgSO4, filtered, and concentrated in vacuo to provide 2.1 g of the titled product as light yellow solid (˜100% yield): [M+H+] m/z 260.
WORKUP
后处理
- temperatureThe mixture was refluxed for 2 hours
- extractionThe aqueous mixture was extracted with DCM (3×)
- dry with materialthe combined organics were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo