Reaktion #2063060

Reaktionsgleichung

1-(3,4-dichlorophenyl)piperazine

5-chloropentanenitrile

sodium carbonate

→

4-(3,4-dichlorophenyl)-1-piperazinepentanenitrile

Ausbeute 72.1%

Lösungsmittel

4-methyl-2-pentanone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 10 hours
2. 2
   TemperaturThe reaction mixture was cooled
3. 3
   Filtrationfiltered
4. 4
   Sonstigethe filtrate was evaporated
5. 5
   SonstigeThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
6. 6
   SonstigeThe pure fractions were collected
7. 7
   Sonstigethe solvent was evaporated

Vorschrift

A mixture of 1-(3,4-dichlorophenyl)piperazine (0.1 mol), 5-chloropentanenitrile (0.13 mol), sodium carbonate (10 g) and potassium iodide (0.1 g) in 4-methyl-2-pentanone (280 ml) was stirred and refluxed for 10 hours. The reaction mixture was cooled, filtered and the filtrate was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5). The pure fractions were collected and the solvent was evaporated, yielding 22.5 g (72%) of 4-(3,4-dichlorophenyl)-1-piperazinepentanenitrile (interm. 2).

Quelle