反应详情

1.87 g of 2-benzylamino-4-(2-methoxyethoxy)-3-nitropyridine (starting material J2) are dissolved in a mixture of 30 ml of methanol and 6.16 ml of 2N aqueous hydrochloric acid and hydrogenated over 500 mg of 10% strength Pd on carbon at 50° C. for 5 hours. After filtration and addition of 6.16 ml of 2N aqueous sodium hydroxide solution the mixture is evaporated to dryness and the residue is chromatographed on silica gel (dichloromethane/methanol 25:1+1% triethylamine). Concentration of the pure fractions and drying in vacuo gives 0.89 g of the title compound as a brownish oil. The mass spectrum shows the molecular peak M+ at 184.0 Da.

1. filtrationAfter filtration and addition of 6.16 ml of 2N aqueous sodium hydroxide solution the mixture
2. customis evaporated to dryness
3. customthe residue is chromatographed on silica gel (dichloromethane/methanol 25:1+1% triethylamine)
4. customConcentration of the pure fractions and drying in vacuo