HRID54923

反应详情

EQUATION

反应方程式

HRID 54923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a freshly prepared solution of sodium ethoxide in ethanol (from 0.35 g sodium metal and 10 ml ethanol) was added 6H-pyrido[3,2,1-de]acridin-1(2H)-one (1.2 g) portionwise over a period of 10 minutes. To the resulting dark red solution was slowly added diethyl carbonate (1.77 g) and the solution was then refluxed for 3 hours. The reaction mixture was cooled, acidified to pH 2 with concentrated HCl and then extracted with methylene chloride. The organic extract was washed with water and was then collected, dried and evaporated to dryness to obtain a light amber solid (1.8 g; m.p. 113°-118° C.).

WORKUP

后处理

  1. temperaturethe solution was then refluxed for 3 hours
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with methylene chloride
  4. extractionThe organic extract
  5. washwas washed with water
  6. customwas then collected
  7. customdried
  8. customevaporated to dryness
  9. customto obtain a light amber solid (1.8 g; m.p. 113°-118° C.)