反应详情

温度

85 °C

151.3 gms (1.4833 mole) of acetic anhydride was added at 45-50° C. to a mixture of 90.0 gm (o.4595 moles) of 4-nitro-2,3,5-trimethylpyridine-N-oxide of formula-IV and 45.0 gms of acetic acid and heated to 85° C. and maintained at the temperature at 85-90° C. for 4 hrs. 75 ml of methanol was added to the reaction mixture at room temperature and distilled off acetic acid and methanol at temperature of 60-65° C. under vacuum to get an oil. 40% Sodium hydroxide solution (240 g) was added to the cooled oil at 0-5°°C. and stirred for 4 hrs. The crude product was obtained by extraction of the reaction mass with methylene chloride and distillation of the solvent. Pure 2-hydroxymethyl-3,5-dimethyl-4-nitropyridine of formula-II was obtained by re-crystallization of the crude material in toluene.

1. temperaturemaintained at the temperature at 85-90° C. for 4 hrs
2. distillationdistilled off acetic acid and methanol at temperature of 60-65° C. under vacuum
3. customto get an oil