反応 #2063060

反応方程式

1-(3,4-dichlorophenyl)piperazine

5-chloropentanenitrile

sodium carbonate

→

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

収率 72.1%

溶媒

4-methyl-2-pentanone

反応条件

後処理

1. 1
   温度refluxed for 10 hours
2. 2
   温度The reaction mixture was cooled
3. 3
   ろ過filtered
4. 4
   その他the filtrate was evaporated
5. 5
   その他The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
6. 6
   その他The pure fractions were collected
7. 7
   その他the solvent was evaporated

実験手順

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).

出典