HRID1197666

反应详情

EQUATION

反应方程式

HRID 1197666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

268 mg (1 mmol) of 4-(3-nitrophenyl)-3-pyridyl-3-butene-2-one, 905 mg (5 mmol) of (2E,4E)-2,4-hexadiene-1-yl 3-aminocrotonate, 273 mg (2 mmol) of zinc chloride, and 500 mg of Molecular Shieves 4A were 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 b 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 182 mg (42.3%).

WORKUP

后处理

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