反应详情

To a solution of 3-(4-Methyl-2-oxo-2H-pyridin-1-yl)-5-nitro-benzoic acid methyl ester (1000 mg, 3.47 mmol) in methanol was added SnCl2 (2.63 g, 13.9 mmol) at room temperature. The reaction mixture was refluxed for 3 hours, then cooled to room temperature. Solvent was removed in vacuo, and the residue was dissolved in H2O and basified by addition of Na2CO3 to pH=9. The mixture was extracted with CH2Cl2, and the combined organic phase was washed with water, brine, and dried over Na2SO4. Solvent was removed under vacuum to give 3-Amino-5-(4-Methyl-2-oxo-2H-pyridin-1-yl)benzoic acid methyl ester (895 mg, 100%) as yellow solid. MS (M+H)=260.

1. temperatureThe reaction mixture was refluxed for 3 hours
2. customSolvent was removed in vacuo
3. dissolutionthe residue was dissolved in H2O
4. additionbasified by addition of Na2CO3 to pH=9
5. extractionThe mixture was extracted with CH2Cl2
6. washthe combined organic phase was washed with water, brine
7. dry with materialdried over Na2SO4
8. customSolvent was removed under vacuum