HRID645377
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe reaction mixture is heated
- temperatureat reflux for 30 minutes
- concentrationconcentrated to dryness
- customThe residue is chromatographed on a column of silica (40-63 μm), elution
- additionbeing carried out with a mixture of dichloromethane and ammoniacal methanol (90/10)
- concentrationconcentrated