反应详情

To a solution N-(4,6-bis-propylamino-[1,3,5]triazin-2-yl)-O-isopropyl-N-methyl-hydroxylamine (LXIV, 1.93 g, 6.83 mmol) in 1,4-dioxane (6 mL) at 0° C. was added 95% H2SO4 (0.36 mL, 6.83 mmol) in a drop-wise manner. The mixture was stirred for 0.5 h at room temperature and then the volatiles were removed under reduced pressure. The residue was co-evaporated with dry toluene (3×25 mL) to yield N-(4,6-bis-propylamino-[1,3,5]triazin-2-yl)-O-isopropyl-N-methyl-hydroxylamine hydrogen sulfate (quantitative yield). 400 MHz 1H-NMR (DMSO-d6, ppm) 11.3-10.7 (1H, br s), 8.8-8.4 (1H, br s), 8.2-8.0 (0.3H, br s), 8.04-7.65 (0.7H, m), 4.43-4.28 (1H, m), 3.42-3.18 (7H, m), 1.64-1.44 (4H, m), 1.25 (6H, d, J=6.1 Hz), 0.94-0.82 (6H, m). ESI-MS (m/z): 283 [M+H]+.

1. customthe volatiles were removed under reduced pressure