HRID2291181

反应详情

EQUATION

反应方程式

HRID 2291181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.8 Grams of 6-(1-oxo-2-piperazinylbutyl)-3,4-dihydrocarbostyril, 2.0 g of p-bromonitrobenzene, 1.2 g of potassium carbonate and 0.1 g of copper powder were dispersed in 80 ml of ethyl cellosolve and stirred at 120°-150° C. by heating for 5 hours. The reaction mixture was concentrated under a reduced pressure and the residue thus obtained was added water and extracted with chloroform. The chloroform layer was washed with water, dried and the chloroform was removed by distillation. The residue thus obtained was separated and purified by a separative thin layer chromatography and recrystallized from ethanol to obtain 0.2 g of 6-{1-oxo-2-[4-(4-nitrophenyl)-1-piperazinyl]-butyl}-3,4-dihydrocarbostyril in yellow powdery crystals.

WORKUP

后处理

  1. temperatureby heating for 5 hours
  2. concentrationThe reaction mixture was concentrated under a reduced pressure
  3. customthe residue thus obtained
  4. extractionextracted with chloroform
  5. washThe chloroform layer was washed with water
  6. customdried
  7. customthe chloroform was removed by distillation
  8. customThe residue thus obtained
  9. customwas separated
  10. custompurified by a separative thin layer chromatography
  11. customrecrystallized from ethanol