反应详情

温度

30 °C

A solution of diethyl 3-(2-(4-hydroxy-2-(pyridazin-3-yl)pyrimidin-5-ylamino)-2-oxoethyl)phenyl-phosphonate (35i, 280 mg, 0.63 mmol) in DCM (20 mL) was added with TMSBr (1.9 g, 12.6 mmol) and stirred at 30° C. for overnight. The reaction mixture was concentrated in vacuum. The residue was added with MeOH (50 mL), stirred for 20 min, and concentrated. The residue was added with water (20 mL) and MeCN (0.5 mL). The solids were filtered to afford the pure product, 35-1, as a white solid (70 mg, 29%). 1H NMR (300 MHz, DMSO) δ 3.9 (s, 2H), 7.39-7.58 (m, 3H), 7.70 (d, J=12.9 Hz, 1H), 7.93 (m, 1H), 8.42 (d, J=8.7 Hz, 1H), 8.86 (m, 1H), 9.40 (d, J=4.2 Hz, 1H), 9.84 (m, 1H), LC-MS (M+H)+ 388.1

1. concentrationThe reaction mixture was concentrated in vacuum
2. additionThe residue was added with MeOH (50 mL)
3. stirringstirred for 20 min
4. concentrationconcentrated
5. additionThe residue was added with water (20 mL) and MeCN (0.5 mL)
6. filtrationThe solids were filtered
7. customto afford the pure product, 35-1