Sulfuric Acid → 1380342-00-6

Participants

Reaction Steps

Concentrated (95%) H2SO4 (0.72 mL, 12.74 mmol) was added in a dropwise manner to a solution of N-(4,6-bis-n-propylamino-[1,3,5]triazin-2-yl)-N,O-dimethyl-hydroxylamine (XXXV, 3.24 g, 12.74 mmol) in 1,4-dioxane (100 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). The resulting white residue was crystallized from ethanol/ethyl ether to yield N-(4,6-bis-n-propylamino-[1,3,5]triazin-2-yl)-N,O-dimethyl-hydroxylamine, hydrogen sulfate (XXXVI, 3.86 g, 86% yield) as a white solid. 1H NMR (400 MHz, DMSO): δ (ppm) 12.0-11.2 (1H, br s), 8.7-8.3 (0.7H, br s), 8.10 (0.3H, br s), 7.8-7.3 (1H, m), 3.78 (3H, s), 3.40-3.20 (7H, m), 1.61-1.45 (4H, m), 0.93-0.84 (6H, m). ESI-MS (m/z) 255 [M+H]+; melting point: 134-135° C.

Provenance & Evidence