반응 #2063060

반응 방정식

1-(3,4-dichlorophenyl)piperazine

5-chloropentanenitrile

sodium carbonate

→

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

수율 72.1%

용매

4-methyl-2-pentanone

반응 조건

후처리

1. 1
   온도refluxed for 10 hours
2. 2
   온도The reaction mixture was cooled
3. 3
   여과filtered
4. 4
   기타the filtrate was evaporated
5. 5
   기타The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
6. 6
   기타The pure fractions were collected
7. 7
   기타the solvent was evaporated

실험 절차

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).

출처