HRID644187

反应详情

EQUATION

反应方程式

HRID 644187 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe reaction was quenched with water (5 mL) and 1 N HCl (10 mL)
  2. extractionthe reaction was extracted with dichloromethane (100 mL)
  3. washThe organic layer was washed with 1 N HCl (10 mL)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated