反应详情

Powdered potassium nitrate (1.82 g, 18 mmol) was added to a stirred solution of 1-[(diethoxyphosphoryl)methyl]-7-trifluoromethyl[1,2,4]triazolo [4,3-a]quinoxalin-4(5H)-one (3.7 g, 9.15 mmol) in 50 ml of conc. sulfuric acid at 0° C. The mixture was stirred at room temperature overnight, and quenched in ice/water (300 g). The aqueous phase was extracted with ethyl acetate (5×100 ml), and the combined organic extracts were dried with anhydrous sodium sulfate, and evaporated. The residue was triturated with ether to give 3.25 g (79%) of the title compound, m.p. 222°-228° C.; 1H-NMR (DMSO-d6): δ 1.20 (t, 6H), 4.10 (quint, 4H), 4.39 (d, 2H), 7.88 (s, 1H), 8.96 (s, 1H), 12.67 (br s, 1H).

1. customquenched in ice/water (300 g)
2. extractionThe aqueous phase was extracted with ethyl acetate (5×100 ml)
3. dry with materialthe combined organic extracts were dried with anhydrous sodium sulfate
4. customevaporated
5. customThe residue was triturated with ether