HRID2200347

反应详情

EQUATION

反应方程式

HRID 2200347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-bromobutanenitrile (1.50 g, 10.17 mmol) in dimethyl formamide (20 ml) were added 1-(4-chlorophenyl)piperazine (2.0 g, 10.17 mmol) and potassium carbonate (2.81 g, 20.34 mmol) at room temperature and the reaction mixture was stirred for 3 h at same temperature. The progress of the reaction was monitored by TLC. The reaction mixture was diluted with water (50 ml) and the aqueous layer was extracted with ethyl acetate (3×50 ml). The combined organic layer was dried over anhydrous sodium sulphate. The solvent in the organic layer was removed under reduced pressure to obtain a crude product, which was purified by column chromatography over silica gel (100-200 mesh) using 10% ethyl acetate in hexane to yield the title compound (2.32 g, 86% yield).

WORKUP

后处理

  1. extractionthe aqueous layer was extracted with ethyl acetate (3×50 ml)
  2. dry with materialThe combined organic layer was dried over anhydrous sodium sulphate
  3. customThe solvent in the organic layer was removed under reduced pressure
  4. customto obtain a crude product, which
  5. customwas purified by column chromatography over silica gel (100-200 mesh)