反应详情

To a solution of 3-(5-methyl-pyridin-2-yl)-5-nitro-benzoic acid methyl ester (4 g, 14.7 mmol) in methanol/ethyl acetate was added SnCl2 (11.15 g, 58.8 mmol) at room temperature. The reaction mixture was refluxed for 3 hours and then cooled. Solvent was removed under reduced pressure and the residue was dissolved in H2O and basified by addition of Na2CO3 to pH=9. The mixture was extracted with CH2Cl2, and the organic phase was washed with water, brine, and dried over Na2SO4. The solvent was removed under reduced pressure to give 3-amino-5-(5-methyl-pyridin-2-yl)-benzoic acid methyl ester (3.2 g, 90%) as white solid.

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