反应详情

To the mixture of 2-chloro-5-fluoropyridine-3-carbonitrile, 2, (29.6 g, 157.1 mmol) in n-butanol (492 mL) was added hydrazine hydrate (76.4 mL, 1.6 mol). This mixture was heated to reflux for 4.5 h and cooled down. n-Butanol was removed under reduced pressure and water (300 mL) was added resulting in a yellow precipitate. The suspension was filtered and washed with water twice, followed by a MTBE wash. The yellow solid was dried in a vacuum oven to give 18 g of the desired product: 1H NMR (300 MHz, d6-DMSO) δ 12.08 (s, 1H), 8.38 (dd, J=2.7, 1.9 Hz, 1H), 7.97 (dd, J=8.8, 2.7 Hz, 1H), 5.56 (s, 2H); LC/MS Gradient 10-90%, 0.1% formic 5 min, C18/ACN, Retention Time=1.25 min, (M+H) 152.95.

1. temperatureThis mixture was heated
2. temperatureto reflux for 4.5 h
3. temperaturecooled down
4. customn-Butanol was removed under reduced pressure and water (300 mL)
5. additionwas added
6. customresulting in a yellow precipitate
7. filtrationThe suspension was filtered
8. washwashed with water twice
9. washwash
10. customThe yellow solid was dried in a vacuum oven