HRID1374889

反应详情

EQUATION

反应方程式

HRID 1374889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

The product from Stage 1 (27.4 g) was treated with a solution of sodium hydroxide (9.6 g) in water (50 ml) then stirred at 90° C. for 1.5 hours. The mixture was cooled to ambient temperature, diluted with water then washed with ethyl acetate. The aqueous phase was separated, acidified with concentrated hydrochloric acid and extracted with ethyl acetate (three times). The extracts were combined, washed with brine and dried over magnesium sulphate. The solvent was evaporated under reduced pressure to give the required product as a pale brown solid, 24.8 g, m.p. 98–101° C.

WORKUP

后处理

  1. temperatureThe mixture was cooled to ambient temperature
  2. washthen washed with ethyl acetate
  3. customThe aqueous phase was separated
  4. extractionextracted with ethyl acetate (three times)
  5. washwashed with brine
  6. dry with materialdried over magnesium sulphate
  7. customThe solvent was evaporated under reduced pressure