HRID2296336

反应详情

EQUATION

反应方程式

HRID 2296336 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.3 g. (0.03 mol) 7-hydroxy-2-methyl-4H-1-benzopyran-4-one are added to a solution of 0.69 g. (0.03 mol) sodium in 75 ml. propan-2-ol and the mixture heated under reflux for 10 minutes. 8.4 g. (0.03 mol) 3-(4-Benzamidopiperidino)-propyl chloride dissolved in 25 ml. propan-2-ol are added thereto, the mixture heated under reflux for 12 hours, evaporated and the residue taken up in dichloromethane and the solution washed with dilute aqueous sodium hydroxide solution. The organic phase is evaporated and the residue recrystallised from propan-2-ol. There are obtained 6.8 g. (54% of theory) 7-[3-(4-benzamidopiperidino)propoxy]-2-methyl-4H-1-benzopyran-2-one; m.p. 173°-175° C.

WORKUP

后处理

  1. temperatureunder reflux for 10 minutes
  2. temperaturethe mixture heated
  3. temperatureunder reflux for 12 hours
  4. customevaporated
  5. washthe solution washed with dilute aqueous sodium hydroxide solution
  6. customThe organic phase is evaporated
  7. customthe residue recrystallised from propan-2-ol
  8. customThere are obtained 6.8 g