反应详情

To a solution of 4′-Methyl-5-nitro-biphenyl-3-carboxylic acid methyl ester (10.00 g, 36.9 mmol) in methanol was added SnCl2 (27.98 g, 147.6 mmol) at room temperature. The reaction mixture was refluxed for 3 hours, then cooled. Solvent was removed in vacuo and the residue was dissolved in H2O, then basified by addition of Na2CO3 to pH=9. The mixture was extracted by CH2Cl2, and the organic phase was washed with water followed by brine, and dried over Na2SO4. The solvent was removed under vacuum to give 5-Amino-4′-methyl-biphenyl-3-carboxylic acid methyl ester (8.48 g, 95%) as yellow oil. MS (M+H)=242.

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