反应详情

20.0 ml of a 30% ethanolic solution of methylamine were added dropwise to a mixture of 29.0 g of 2,6-dichloro-3-nitropyridine, 300 ml of ethanol and 36.6 g of sodium carbonate, whilst cooling with ice, and the resulting mixture was stirred at room temperature for 8 hours. At the end of this time, the reaction mixture was freed from ethanol by distillation. The residue was diluted with water, after which it was extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, after which the solvent was removed by distillation under reduced pressure. The residue was crystallized by trituration with ethanol, to give 22.3 g of the title compound, melting at 114° C.

1. temperaturewhilst cooling with ice
2. distillationAt the end of this time, the reaction mixture was freed from ethanol by distillation
3. additionThe residue was diluted with water
4. extractionafter which it was extracted with ethyl acetate
5. washThe extract was washed with an aqueous solution of sodium chloride
6. dry with materialdried over anhydrous sodium sulfate
7. customafter which the solvent was removed by distillation under reduced pressure
8. customThe residue was crystallized by trituration with ethanol