反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 liquid 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)-piperazinyl]butyl}-3,4-dihydrocarbostyril in yellow powdery crystals.
WORKUP
后处理
- temperaturerefluxed
- temperatureby heating for 5 hours
- filtrationThe reaction mixture was filtered
- concentrationthe mother liquid was concentrated by distillation under a reduced pressure to dryness
- customThe residue thus obtained
- extractionwas extracted with methanol-chloroform
- customthe solvent was removed by distillation
- customto obtain a residue
- customThe residue was purified
- customseparated by a preparative silica-gel thin layer chromatograph