反应 #2063060

ord-4a5bdc30be874aee83bdc8629aaa3da8

反应方程式

Clc1ccc(N2CCNCC2)cc1Cl
1-(3,4-dichlorophenyl)piperazine
N#CCCCCCl
5-chloropentanenitrile
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
N#CCCCCN1CCN(c2ccc(Cl)c(Cl)c2)CC1
4-(3,4-dichlorophenyl)-1-piperazinepentanenitrile
收率 72.1%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06224849B1uspto-grants-2001_05