HRID1452318

反应详情

EQUATION

反应方程式

HRID 1452318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 4.24 g of 8-carboxy-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran and 6.3 g of anhydrous potassium carbonate in 60 ml of dimethylformamide was stirred at 80° C. for 30 minutes. 5.23 g of 1-(3-chloropropyl)-4-(2-methoxyphenyl)-piperazine was then added and stirring was continued at 80° C. for 3.5 hours. The reaction mixture was cooled to ambient temperature, poured on to iced water and extracted with ethyl acetate. The organic extracts were washed with aqueous sodium chloride solution, dried on anhydrous sodium sulfate, and evaporated to dryness in vacuo. The residue was taken up in ethanol and excess ethanolic hydrogen chloride was added to the solution. Yield: 8.16 g of the title compound, m.p. 198°-203° C.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued at 80° C. for 3.5 hours
  3. temperatureThe reaction mixture was cooled to ambient temperature
  4. extractionextracted with ethyl acetate
  5. washThe organic extracts were washed with aqueous sodium chloride solution
  6. dry with materialdried on anhydrous sodium sulfate
  7. customevaporated to dryness in vacuo
  8. additionexcess ethanolic hydrogen chloride was added to the solution