反应详情

95% H2SO4 (0.26 mL, 4.62 mmol) was added dropwise to the solution of 6-(N,N′-dimethyl-hydrazino)-N,N′-dipropyl-[1,3,5]triazine-2,4-diamine (XLIX) (1.17 g, 4.62 mmol) in 1,4-dioxane (10 mL) at 0° C. The mixture was stirred for 0.5 h at room temperature; 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)-N,N′-dimethyl-hydrazine hydrogen sulfate (L) in quantitative yield. 400 MHz 1H NMR (DMSO-d6, ppm) 8.48-8.32 (1H, m), 7.9-7.7 (0.5H, br s), 7.70-7.61 (0.5H, m), 3.34-3.20 (4H, m), 3.21 (1.5H, s), 3.17 (1.5H, s), 2.52 (1.5H, s), 2.51 (1.5H, s, overlapped with DMSO), 1.59-1.46 (4H, m), 0.93-0.82 (6H, m). ESI-MS (m/z): 254 [M+H]+.

1. customvolatiles were removed under reduced pressure