反应详情

N-(4,6-bis-n-propylamino-[1,3,5]triazin-2-yl)-O-(2,2-difluoro-ethyl)-hydroxylamine (C, 1.02 g, 3.51 mmol) was reacted with 95% H2SO4 (0.19 mL, 3.51 mmol) in diethyl ether (3 mL) at 0° C. Two drops of EtOH were added, and the resultant crystals were filtered, washed with diethyl ether, and dried to yield N-(4,6-bis-n-propylamino-[1,3,5]triazin-2-yl)-O-(2,2-difluoro-ethyl)-hydroxylamine hydrogen sulfate (CI) (1.26 g, 93%). 400 MHz 1H NMR (DMSO-d6, ppm) 11.8-10.5 (1H, m) 8.8-8.4 (0.3H, br s) 8.36-7.53 (1.7H, m) 6.50-6.08 (1H, m) 4.28-4.07 (2H, m) 3.39-3.13 (4H, m) 1.64-1.42 (4H, m) 0.97-0.78 (6H, m). ESI-MS (m/z) 291 [M+H]+. M.P.: 91-93° C.

1. filtrationthe resultant crystals were filtered
2. washwashed with diethyl ether
3. customdried