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To a solution of 5.012 g (72.1 mmol) of hydroxylamine hydrochloride in 55 mL of isopropyl alcohol, 8.8 g (105.7 mmol) of sodium bicarbonate was added. The resulting mixture was stirred at 25° C. to 30° C. for 10-15 min. 5.0 g (48 mmol) of 3-cyanopyridine was added and stirred at 80° C. to 85° C. for 3-4 h. After completion of the reaction, the reaction mixture was cooled to 25° C. to 30° C., filtered and washed with 10 mL of isopropyl alcohol. The filtrate was collected and distilled to obtain a crude residue, which was chased with 5 mL of toluene to yield the title compound.

1. stirringstirred at 80° C. to 85° C. for 3-4 h
2. customAfter completion of the reaction
3. temperaturethe reaction mixture was cooled to 25° C. to 30° C.
4. filtrationfiltered
5. washwashed with 10 mL of isopropyl alcohol
6. customThe filtrate was collected
7. distillationdistilled
8. customto obtain a crude residue, which