HRID645377

反应详情

EQUATION

反应方程式

HRID 645377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The N,N-dimethyl-6-nitropyridine-3-amine obtained above is taken up in 25 ml of ethanol. After addition of 4.8 g of stannous chloride, the reaction mixture is heated at reflux for 30 minutes and then concentrated to dryness. The residue is chromatographed on a column of silica (40-63 μm), elution being carried out with a mixture of dichloromethane and ammoniacal methanol (90/10). The fractions comprising the expected product are combined and concentrated to give 750 mg of 5-dimethylaminopyridine-2-amine in the form of a pasty yellow solid.

WORKUP

后处理

  1. temperaturethe reaction mixture is heated
  2. temperatureat reflux for 30 minutes
  3. concentrationconcentrated to dryness
  4. customThe residue is chromatographed on a column of silica (40-63 μm), elution
  5. additionbeing carried out with a mixture of dichloromethane and ammoniacal methanol (90/10)
  6. concentrationconcentrated