反应详情

To a solution of methyl 2-(3-chloro-7-hydroxy-2,5-di-methylpyrazolo[1,5-a]pyrimidin-6-yl)acetate (0.160 g, 0.6 mmol) was added POCl3 (1 mL). 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 were 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 (0.1 g, 59%). NMR (500 MHz, DMSO-d6) δ ppm 2.44 (s, 3H), 2.57 (s, 3H), 3.68 (s, 3H), 4.00 (s, 2H). Used as is in the next step.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 1 h
3. temperatureAfter cooling
4. customA brown solid precipitated
5. filtrationThe solid were 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