HRID1178300

反应详情

EQUATION

反应方程式

HRID 1178300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 21.6 g of the compound of Step A above in 48 ml of Claisen's alkali solution (solution of 21 g of KOH in 15 ml of water, made up to 60 ml with methanol) is heated at reflux for 4 hours. The reaction mixture is then diluted with 50 ml of water and poured into 75 ml of 15.5% hydrochloric acid solution cooled to 0° C. with stirring. The white precipitate formed is then filtered off over a Buchner funnel and then washed with water and dried under a phosphoric vacuum. The dry residue obtained is dissolved in a solution of ethanol and water (80:20, v/v) at boiling. After cooling to 0° C., 13.7 g of the expected product are obtained.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureat reflux for 4 hours
  3. customThe white precipitate formed
  4. filtrationis then filtered off over a Buchner funnel
  5. washwashed with water
  6. customdried under a phosphoric vacuum
  7. customThe dry residue obtained
  8. temperatureAfter cooling to 0° C.