反应详情

Hydroxylamine (58.5 g, 842 mmol) and N,N-diisopropylethylamine (65.3 g, 86.3 mL, 505 mmol) were dissolved in methanol (200 mL) and ethanol (200 mL). N-(3-Bromo-pyridin-2-yl)-N′-ethoxycarbonyl-thiourea (51.2 g, 168 mmol) was added and the reaction mixture was stirred at room temperature for 1 hour and then at 60° C. for 3 hours. The white precipitate was filtered off and triturated with water for 25 minutes, filtered and triturated two times with diethylether. The solid was dried by co-evaporation with toluene and dried in vacuum. The title compound was obtained as a white solid (27.9 g, 78%).

1. waitat 60° C. for 3 hours
2. filtrationThe white precipitate was filtered off
3. customtriturated with water for 25 minutes
4. filtrationfiltered
5. customtriturated two times with diethylether
6. dry with materialThe solid was dried by co-evaporation with toluene
7. customdried in vacuum