反应详情

Toluene-4-sulfonic acid 5acetyl-4-(2-fluorophenyl)-1H-pyrazol-3-yl ester (1.0 g, 2.7 mmol; prepared as described in Example 1, steps a to c) was stirred with benzhydrazide (400 mg, 2.9 mmol) in xylene (30 ml) at reflux overnight. The mixture was allowed to cool to room temperature. A solid crystallised out of solution This was separated by filtration, and was recrystallised from ethyl acetate, yielding toluene-4-sulfonic acid 3-(2-fluorophenyl)-4-methyl-7-phenylpyrazolo[1,5-d][1,2,4]triazin-2-yl ester as a white solid (694 mg). 1H NMR (400 MHz, CDCl3) δ 2.47 (3H, s), 2.52 (3H, s), 7.19 (1H, t, J=8.9 Hz), 7.28 (3H, m), 7.41-7.52 (4H, m), 7.61 (1H, m), 7.79 (2H, d, J=8.3 Hz), 8.25 (2H, d, J=7.5 Hz); MS (ES+) m/e 475 [MH]+.

1. customprepared
2. temperatureat reflux overnight
3. customA solid crystallised out of solution
4. customThis was separated by filtration
5. customwas recrystallised from ethyl acetate