HRID1197667

反应详情

EQUATION

反应方程式

HRID 1197667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixuture of 0.536 g (2 mmol) of 4-(3-nitrophenyl)-3-pyridyl-3-butene-2-one, 0.821 g (10 mmol) of 3-aminocrotonitrile, 0.546 g (4 mmol) of zinc chloride, and 1.0 g of Molecular Shieves 4A was added to 1,4-dioxane. This reaction mixture was refluxed with application of heat in an inert atmoshpere for 5 hours. The reaction mixture was then cooled to room temperature and neutralized with a saturated aqueous solution of sodium hydrogencarbonate, followed by extraction with chloroform. The solvents contained in the extract were distilled off and the residue was chromatographed on a silica gel column, whereby the captioned compound was obtained. The yield was 0.59 g (84.6%).

WORKUP

后处理

  1. temperatureThis reaction mixture was refluxed with application
  2. temperatureof heat in an inert atmoshpere for 5 hours
  3. extractionfollowed by extraction with chloroform
  4. distillationwere distilled off
  5. customthe residue was chromatographed on a silica gel column, whereby the captioned compound
  6. customwas obtained