反应详情

A mixture of 4-[2-amino-6-(2-{4-[3-(methyloxy)phenyl]-1H-imidazol-2-yl}-4-morpholinyl)-4-pyrimidinyl]-2-fluorobenzonitrile (700 mg, 1.485 mmol) and hydrazine (2.35 mL, 74.2 mmol) in ethanol (8.0 mL) was heated under microwave conditions with stirring for 1 hour. The mixture was concentrated, and water (20 mL) was added. The resulting mixture was filtered to afford the crude title compound (725 mg) as a yellow solid. This material was combined with another sample of the title compound (25 mg). The combined material was washed with CH2Cl2 (2×25 mL) and EtOAc (2×20 mL), and dried under high vacuum to afford the title compound (216 mg) as a yellow solid. LC-MS (ES) m/z=484 [M+H]+. 1H NMR (400 MHz, DMSO-d6): δ 3.08-3.15 (m, 1H), 3.23 (d, J=8.8 Hz, 1H), 3.69-3.76 (m, 1H), 3.79 (s, 3H), 4.05 (d, J=11.2 Hz, 1H), 4.33 (d, J=9.6 Hz, 1H), 4.62 (dd, J=10.0 Hz, 2.4 Hz, 1H), 4.73 (s, 1H), 5.38 (s, 2H), 6.21 (s, 2H), 6.71 (s, 1H), 6.76 (d, J=8.2 Hz, 1H), 7.25 (t, J=8.0 Hz, 1H), 7.35-7.37 (m, 2H), 7.54-7.63 (m, 2H), 7.71 (d, J=8.4 Hz, 1H), 7.97 (s, 1H), 11.52 (s, 1H), 12.34 (s, 1H).

1. temperaturewas heated under microwave conditions
2. concentrationThe mixture was concentrated
3. additionwater (20 mL) was added
4. filtrationThe resulting mixture was filtered
5. customto afford the crude title compound (725 mg) as a yellow solid