HRID639232

反应详情

EQUATION

反应方程式

HRID 639232 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 4-bromo-3-hydroxybenzoic acid (30 mmol) in methanol (100 mL) was added concentrated sulfuric acid (2.6 mL). The solution was heated at reflux for 5 hours, cooled to 0° C., and then brought to pH 7 by adding saturated aqueous sodium carbonate. The solution was evaporated to one-third the original volume. Water was added and the product was extracted into ethyl acetate. The organic extracts were washed with water and brine and dried over anhydrous sodium sulfate. Evaporation gave 6.15 g (89%) of the product as a white solid, m.p. 130-132° C.

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureat reflux for 5 hours
  3. customThe solution was evaporated to one-third the original volume
  4. additionWater was added
  5. extractionthe product was extracted into ethyl acetate
  6. washThe organic extracts were washed with water and brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. customEvaporation