HRID329881

反应详情

EQUATION

反应方程式

HRID 329881 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 1-piperazineethanol (11.4 g), potassium carbonate powder (24.3 g) and N,N-dimethylformamide (100 ml) was added dropwise benzhydryl bromide (21.7 g) under stirring. The mixture was stirred at room temperature for 2 hours, diluted with water and extracted with ethyl ether. The ethyl ether layer was washed with saturated aqueous sodium chloride and dried over anhydrous sodium sulfate. The solvent was then distilled off and the residue was purified by silica gel chromatography [eluent: hexane-ethyl acetate (2:1)] to give 21.9 g (84.2%) of 4-benzhydryl-1-piperazineethanol as an oil. IR(Neat): 3380 cm-1. NMR(CDCl3)δ: 2.46(10H, broad s), 3.57(2H, t, J=6.5), 4.20(1H, s), 7.03-7.45(12H, m).

WORKUP

后处理

  1. stirringThe mixture was stirred at room temperature for 2 hours
  2. extractionextracted with ethyl ether
  3. washThe ethyl ether layer was washed with saturated aqueous sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was then distilled off
  6. customthe residue was purified by silica gel chromatography [eluent: hexane-ethyl acetate (2:1)]