Reaktion #657148

Reaktionsgleichung

ammonia water

5-[2-hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydrocarbostyril

acetone

acetyl chloride

→

5-[2-acetyloxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydrocarbostyril

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONare added
2. 2
   Temperaturby heating for 10 hours under refluxing conditions
3. 3
   TemperaturAfter cooling the reaction mixture
4. 4
   Sonstigethe product precipitated
5. 5
   Filtrationis collectd by filtration
6. 6
   Waschenwashed with acetone
7. 7
   SonstigeThe crude crystals thus obtained
8. 8
   Extraktionextracted with chloroform
9. 9
   Sonstigedried
10. 10
    Sonstigechloroform is removed by distillation
11. 11
    SonstigeThe residue is purified by silica gel chromatography

Vorschrift

2 Grams of 5-[2-hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydrocarbostyril are mixed with 30 ml of acetone and further 12 ml of acetyl chloride are added followed by heating for 10 hours under refluxing conditions. After cooling the reaction mixture, the product precipitated is collectd by filtration and washed with acetone. The crude crystals thus obtained are dissolved in 80 ml of water and made basic with ammonia-water, then extracted with chloroform, dried and chloroform is removed by distillation. The residue is purified by silica gel chromatography to obtain 0.5 g of 5-[2-acetyloxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydrocarbostyril in the form of colorless crystals with a melting point of 159°-161° C.

Quelle