Reaktion #2378365

Reaktionsgleichung

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

p-bromonitroaniline

potassium carbonate

→

3,4-dihydrocarbostyril

Lösungsmittel

3-methoxybutanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed
2. 2
   Temperaturby heating for 5 hours
3. 3
   FiltrationThe reaction mixture was filtered
4. 4
   Einengenthe mother liquor was concentrated by distillation under a reduced pressure to dryness
5. 5
   SonstigeThe residue thus obtained
6. 6
   Extraktionwas extracted with methanol-chloroform
7. 7
   Sonstigethe solvent was removed by distillation
8. 8
   Sonstigeto obtain a residue
9. 9
   SonstigeThe residue was purified
10. 10
    Sonstigeseparated by a preparative silica-gel thin layer chromatograph

Vorschrift

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.

Quelle