反应详情

温度

70 °C

To a mechanically stirred suspension of 2-isonicotinoyl-N-methylhydrazinecarbothioamide (610 g) in water (5.0 L) was added sodium bicarbonate (390 g) at r.t. The reaction mixture was thereafter slowly heated to 70° C. over 2 h, and maintained at that temperature for another 3.5 h before cooling (ice-bath) to 17° C., followed by adjusting the pH to 3 by slow addition (over 90 min) of concentrated hydrochloric acid (ca. 470 mL). Subsequent filtration of the reaction mixture, followed by washing the collected solid with dilute hydrochloric acid (0.1 N, 2×1.0 L), gave a wet cake that was dried at 100 mbar under a gentle stream of air for 1.5 days to yield 544 g of the title compound.

1. temperaturemaintained at that temperature for another 3.5 h
2. temperaturebefore cooling (ice-bath) to 17° C.
3. filtrationSubsequent filtration of the reaction mixture
4. washby washing the collected solid with dilute hydrochloric acid (0.1 N, 2×1.0 L)
5. customgave a wet cake that
6. customwas dried at 100 mbar under a gentle stream of air for 1.5 days