反应详情

温度

80 °C

In a 25 mL flask under argon was added 4-[2-amino-6-(ethylamino)-4-pyrimidinyl]-2-fluorobenzonitrile (0.164 g, 0.442 mmol) followed by EtOH (3.5 mL). Hydrazine monohydrate (0.87 mL, 17.7 mmol) was added and the reaction mixture was stirred for 6 hours at 80° C. The reaction was cooled to room temperature and concentrated to near dryness. Water (3 mL) was added (orange oil was formed) followed by CH3CN (8 drops), and the mixture was sonicated. A light yellow precipitate was formed. The suspension was cooled on an ice bath and the solid was filtered, washed with water and dried under vacuum at 40° C. to afford the title compound (82 mg, 68%) as a light yellow solid. LC-MS (ES) m/z=270 [M+H]+. 1H NMR (400 MHz, DMSO-d6): δ 1.13 (t, J=7.2 Hz, 3H), 3.20-3.40 (m, 2H), 5.36 (s, 2H), 5.97 (s, 2H), 6.25 (s, 1H), 6.82 (bs, 1H), 7.41 (d, J=8.3 Hz, 1H), 7.69 (d, J=8.3 Hz, 1H), 7.84 (s, 1H), 11.50 (s, 1H).

1. temperatureThe reaction was cooled to room temperature
2. concentrationconcentrated
3. additionWater (3 mL) was added
4. custom(orange oil was formed)
5. customthe mixture was sonicated
6. customA light yellow precipitate was formed
7. temperatureThe suspension was cooled on an ice bath
8. filtrationthe solid was filtered
9. washwashed with water
10. customdried under vacuum at 40° C.