HRID1588743

反应详情

EQUATION

反应方程式

HRID 1588743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

59.8 ml (0.50 mole) of tin tetrachloride are added gradually to a solution of 44.5 g (0.2 mole) of 2-n-butyl 5-nitro benzofuran and 44.3 g (0.26 mole) of anisoyl chloride in 308 ml of dichloroethane. The temperature is maintained at 23° C. and stirring is continued for 24 hours. The mixture is poured onto 770 ml of ice-water and extracted 3 times with 150 ml of dichloroethane. The solution is washed with water, 5% sodium hydrogen carbonate solution and again with water. It is evaporated to dryness and the product thus obtained crystallizes rapidly [purity on high performance liquid chromatography (HPLC): 91.69%]. It is recrystallized from 250 ml of isopropanol and 59 g of 2-n-butyl 3-(4-methoxy benzoyl) 5-nitro benzofuran are thus obtained.

WORKUP

后处理

  1. extractionextracted 3 times with 150 ml of dichloroethane
  2. washThe solution is washed with water, 5% sodium hydrogen carbonate solution and again with water
  3. customIt is evaporated to dryness
  4. customthe product thus obtained
  5. customcrystallizes rapidly [purity on high performance liquid chromatography (HPLC): 91.69%]
  6. customIt is recrystallized from 250 ml of isopropanol and 59 g of 2-n-butyl 3-(4-methoxy benzoyl) 5-nitro benzofuran
  7. customare thus obtained