反应详情

温度

100 °C

5-Bromo-6-methylpicolin-imido-hydrazide (1 equiv) and formic acid (15 equiv) were combined and heated with stirring at 100° C. for 6 h. The reaction was cooled to room temperature and diluted with methanol. The resulting slurry was stirred for 30 min and then partially concentrated under reduced pressure to ˜20% of the total volume. The resulting mixture was again diluted with methanol and partially concentrated under reduced pressure to ˜20% of the total volume. The resulting solids were collected by filtration, washed three times with water and dried under reduced pressure to provide the desired product in 84% yield, as an off-white solid. MS (ESI) m/z 238.9 [M]+, 240.9 [M+2]+.

1. temperatureheated
2. temperatureThe reaction was cooled to room temperature
3. stirringThe resulting slurry was stirred for 30 min
4. concentrationpartially concentrated under reduced pressure to ˜20% of the total volume
5. additionThe resulting mixture was again diluted with methanol
6. concentrationpartially concentrated under reduced pressure to ˜20% of the total volume
7. filtrationThe resulting solids were collected by filtration
8. washwashed three times with water
9. customdried under reduced pressure