反应详情

To 2-fluoro-4-iodonicotinaldehyde (11.33 g, 45.1 mmol) in THF (200 mL) was added hydrazine (5.67ml, 181 mmol) dropwise. The resulting mixture was stirred at RT under a nitrogen atmosphere for 5 h. The reaction was concentrated, diluted with 10:1 acetone/MeOH and filtered through a pad of silica gel. Removed most of the solvent in vacuo, then diluted with some hexanes and filtered resulting solid. Dried to yield 4-iodo-1H-pyrazolo[3,4-b]pyridine as an off-white solid. MS m/z=246 [M+1]+. Calc'd for C6H4IN3: 245.02.

1. concentrationThe reaction was concentrated
2. additiondiluted with 10:1 acetone/MeOH
3. filtrationfiltered through a pad of silica gel
4. customRemoved most of the solvent in vacuo
5. additiondiluted with some hexanes
6. filtrationfiltered
7. customresulting solid
8. customDried