HRID1975878

反应详情

EQUATION

反应方程式

HRID 1975878 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

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).

WORKUP

后处理

  1. temperaturerefluxed for 10 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. customthe filtrate was evaporated
  5. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
  6. customThe pure fractions were collected
  7. customthe solvent was evaporated