反应详情

温度

70 °C

A mixture of ethyl [1-({3-amino-5-[4-(6,6-dimethyl-5,6,7,8-tetrahydroquinazolin-4-yl)-2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl]pyridine-2-yl}amino)ethenyl]carbamate (82 mg, 0.15 mmol) and mercury(II) oxide (33 mg, 0.15 mmol) in tetrahydrofuran (8 mL) was stirred at 70° C. for 24 h. On cooling to room temperature, the mixture filtered then concentrated and the residue purified by preparative reverse phase HPLC to afford the title Compound (6 mg, 3% yield over 2 steps) as a colorless solid. 1H NMR (400 MHz, methanol-d4): 8.51 (s, 1H), 8.49 (d, 1H), 8.22 (d, 1H), 7.72 (d, 1H), 7.66 (dd, 1H), 7.09 (d, 1H), 5.17 (s, 2H), 4.48 (m, 2H), 4.36 (q, 2H), 4.33 (m, 2H), 2.85 (m, 2H), 2.60 (s, 2H), 1.69 (m, 2H), 1.38 (t, 3H), 0.95 (s, 6H); MS (EI) for C28H31N7O3: 514 (MH+).

1. temperatureOn cooling to room temperature
2. filtrationthe mixture filtered
3. concentrationthen concentrated
4. customthe residue purified by preparative reverse phase HPLC