HRID981171

反应详情

EQUATION

反应方程式

HRID 981171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-(3-nitrophenyl)-1-phenyl-2-propen-1-one (20 g) and N-(2-morpholinoethyl)-3-aminocrotonamide (21.9 g) in toluene (200 ml) was refluxed for 5 hours. After allowing to cool at ambient temperature, the reaction mixture was concentrated in vacuo. The residue was subjected to a column chromatography on silica gel eluting with a mixture of ethyl acetate and tetrahydrofuran (100:1 V/V). The fractions containing the object compound were combined and concentrated in vacuo. The residue was recrystallized from ethyl alcohol to give 3-(2-morpholinoethylcarbamoyl)-2-methyl-4-(3-nitrophenyl)-6-phenylpyridine (11.0 g, yield 31.2 %).

WORKUP

后处理

  1. temperaturewas refluxed for 5 hours
  2. concentrationthe reaction mixture was concentrated in vacuo
  3. additionThe residue was subjected to a column chromatography on silica gel eluting with a mixture of ethyl acetate and tetrahydrofuran (100:1 V/V)
  4. additionThe fractions containing the object compound
  5. concentrationconcentrated in vacuo
  6. customThe residue was recrystallized from ethyl alcohol