HRID644187
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- -65 °C
PROCEDURE
实验过程
2-Methoxy-4-(methylthio)benzoic acid (1.002 g, 5.05 mmol) was dissolved in dichloromethane (18 mL). The solution was cooled to −65° C. in a dry ice/chloroform bath. A dichloromethane solution of boron tribromide (5.4 mL, 5.4 mmol) was then added slowly. After 3 hours, the reaction was quenched with water (5 mL) and 1 N HCl (10 mL). After stirring for 10 minutes, the reaction was extracted with dichloromethane (100 mL). The organic layer was washed with 1 N HCl (10 mL) and then dried over magnesium sulfate, filtered, and concentrated to give the pure product as a pale yellow solid (866 mg, 4.70 mmol, 93%).
WORKUP
后处理
- customthe reaction was quenched with water (5 mL) and 1 N HCl (10 mL)
- extractionthe reaction was extracted with dichloromethane (100 mL)
- washThe organic layer was washed with 1 N HCl (10 mL)
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated