반응 #1372622

반응 방정식

6-(1-hydroxy-2-piperazinylbutyl)-3,4-dihydrocarbostyril

p-bromonitroaniline

potassium carbonate

→

3,4-dihydrocarbostyril

용매

3-methoxybutanol

반응 조건

후처리

1. 1
   온도refluxed
2. 2
   온도by heating for 5 hours
3. 3
   여과The reaction mixture was filtered
4. 4
   농축the mother liquor was concentrated by distillation under a reduced pressure to dryness
5. 5
   기타The residue thus obtained
6. 6
   추출was extracted with methanol-chloroform
7. 7
   기타the solvent was removed by distillation
8. 8
   기타to obtain a residue
9. 9
   기타The residue was purified
10. 10
    기타separated by a preparative silica-gel thin layer chromatograph

실험 절차

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.

출처