反应详情

The title compound was prepared according to the general procedure as described in method A for the preparation of phosphate derivatives by coupling reaction of N-{4-[2,4-difluoro-3-(trifluoromethyl)phenyl]-1,3-thiazol-2-yl}-2-(1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidin-5-yl)acetamide (3.10 g, 3.01 mmol) with freshly prepared di-tert-butyl iodomethyl phosphate (intermediate 2) (4.20 g, 12.02 mmol in presence of sodium hydride (60% dispersion in mineral oil, 360 mg, 9.01 mmol) in dry DMF (31 ml) to yield 2.45 g of pure product as an off-white solid; 1H NMR (300 MHz, CDCl3): δ 1.46 (s, 18H), 3.34 (s, 3H), 3.57 (s, 3H), 4.43 (s, 2H), 6.43 (d, J=7.8 Hz, 2H), 6.79 (s, 1H), 7.08 (t, J=9.0 Hz, 1H), 7.47 (s, 1H), 8.48 (q, J=8.7 Hz, 1H); ESI (m/z): 738.05 (M+H)+.