反应详情

To methyl 2-(5-methyl-7-oxo-2-phenyl-4,7-dihydropyrazolo[1,5-a]pyrimidin-6-yl)acetate (3 g, 10.09 mmol) was added POCl3 (25 mL, 268 mmol). The reaction mixture was heated at reflux for 1 h. After cooling, the reaction mixture was added drop-wise to ice-water. A brown solid precipitated. The solid was filtered and washed with water, then dissolved in ethyl acetate. The organic solution was washed with saturated NaHCO3 and dried over sodium sulfate. The solvent was evaporated to give the title compound (2.77 g, 84%). 1H-NMR (400 MHz, DMSO-d6) δ ppm 2.58 (3H, s), 3.71 (3H, s), 4.04 (2H, s), 7.29 (1H, s), 7.43-7.58 (3H, m), 8.07 (2H, d, J=7.0 Hz).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 1 h
3. temperatureAfter cooling
4. customA brown solid precipitated
5. filtrationThe solid was filtered
6. washwashed with water
7. dissolutiondissolved in ethyl acetate
8. washThe organic solution was washed with saturated NaHCO3
9. dry with materialdried over sodium sulfate
10. customThe solvent was evaporated