HRID639233

反应详情

EQUATION

反应方程式

HRID 639233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 4-bromo-3-hydroxybenzoate of Step A (27 mmol), potassium carbonate (33 mmol), and dimethyl sulfate (32 mmol) in acetone (40 mL) was stirred at reflux temperature under nitrogen atmosphere for three hours. The mixture was cooled and 5 mL of water was added. The acetone was evaporated and 30 mL of water was added. The product was extracted into dichloromethane. The organic solution was dried over anhydrous magnesium sulfate, filtered and evaporated to give the title compound (6.5 g, 99%) as a hard, white crystalline solid.

WORKUP

后处理

  1. temperatureat reflux temperature under nitrogen atmosphere for three hours
  2. temperatureThe mixture was cooled
  3. customThe acetone was evaporated
  4. addition30 mL of water was added
  5. extractionThe product was extracted into dichloromethane
  6. dry with materialThe organic solution was dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customevaporated