反应详情

温度

70 °C

A suspended mixture of 5-bromo-2-(3-ethylureido)isonicotinamide (Intermediate 5, 237 g, 830 mmol), Lawesson's Reagent (336 g, 830 mmol), and tetrahydrofuran (3 L) was stirred at 70° C. for 18 h. The precipitate was collected by filtration and washed with methyl tert-butyl ether (2×500 L). This solid was then dried in the vacuum oven at 50° C. for 12 h to give 192 g (77%) of 5-bromo-2-(3-ethylureido)pyridine-4-carbothioamide as an off white solid.

1. filtrationThe precipitate was collected by filtration
2. washwashed with methyl tert-butyl ether (2×500 L)
3. customThis solid was then dried in the vacuum oven at 50° C. for 12 h