HRID1978497

反应详情

EQUATION

反应方程式

HRID 1978497 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.362 g (0.878 mM) of (E)-5-(piperidin-4-yl]-1-(5-thia-1,8b-diazaacenaphthylen-4-yl)-1-penten-3-one dihydrochloride, 0.26 g (1.32 mM) of 1-bromo-3-phenylpropane, and 0.43 ml (3.07 mM) of triethylamine in 30 ml of ethanol was refluxed for 1 day. The reaction mixture was then poured in aqueous solution of sodium hydrogen carbonate and extracted with 3 portions of ethyl acetate. The organic layers were pooled and dried over MgSO4 and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate to ethyl acetate/methanol : 9/1) to provide the title compound.

WORKUP

后处理

  1. extractionextracted with 3 portions of ethyl acetate
  2. dry with materialdried over MgSO4
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate to ethyl acetate/methanol : 9/1)