HRID1285440

反应详情

EQUATION

反应方程式

HRID 1285440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.0 Grams of 6-(1-hydroxy-2-piperazinylbutyl)-3,4-dihydrocarbostyril, 3.5 g of p-bromonitroaniline, 1.8 g of potassium carbonate and 0.2 g of copper powder were mixed in 60 ml of 3-methoxybutanol and refluxed by heating for 5 hours. The reaction mixture was filtered and the mother liquor was concentrated by distillation under a reduced pressure to dryness. The residue thus obtained was extracted with methanol-chloroform and the solvent was removed by distillation to obtain a residue. The residue was purified and separated by a preparative silica-gel thin layer chromatograph to obtain 0.21 g of 6-{1-hydroxy-2-[4-nitrophenyl)-1-piperazinyl]butyl}-3,4-dihydrocarbostyril in yellow powdery crystals.

WORKUP

后处理

  1. temperaturerefluxed
  2. temperatureby heating for 5 hours
  3. filtrationThe reaction mixture was filtered
  4. concentrationthe mother liquor was concentrated by distillation under a reduced pressure to dryness
  5. customThe residue thus obtained
  6. extractionwas extracted with methanol-chloroform
  7. customthe solvent was removed by distillation
  8. customto obtain a residue
  9. customThe residue was purified
  10. customseparated by a preparative silica-gel thin layer chromatograph