反应详情

To a stirred solution of 7.46 g (47.51 mmol) of 1-(2,6-difluoropyridin-3-yl)ethanone (37-2) in 50 mL of CH2Cl2 under nitrogen was added dropwise titanium (IV) isopropoxide. The resulting solution was stirred vigorously for 15 minutes before hydrazine hydrate (4.62 g, 95.0 mmol) was added slowly to form a thick slurry. The reaction mixture was stirred for 1 hour before the addition of 11 mL of H2O, and the resulting mixture stirred for 1.5 hours until completion as determined by LC/MS analysis. The solid matter was filtered off and the filterate was condensed to yield a white solid. EtOH (100 mL) was added to the crude intermediate and the mixture was heated to reflux for 6 hours. After the reaction was complete as determined by LC/MS analysis the solvent was removed to yield the desired product. No further purification was necessary. 1H NMR (CDCl3): 2.56 (s, 3H), 6.78 (d, 1H), 8.08 (t, 1H).

1. additionwas added slowly
2. customto form a thick slurry
3. filtrationThe solid matter was filtered off
4. customcondensed
5. customto yield a white solid
6. temperaturethe mixture was heated
7. temperatureto reflux for 6 hours
8. customwas removed