反应详情

温度

90 °C

To a solution of 2-(4-fluorophenyl)-5-methyl-thiazolo[5,4-d]pyrimidin-7(6H)-one (0.40 g, 1.23 mmol) in POCl3 was added diisopropylethylamine (0.13 ml, 0.77 mmol). The reaction mixture was stirred under N2 at 90° C. for 3.5 hours. After cooling down to room temperature, the reaction mixture was poured into ice-water and the aqueous phase was extracted with diethyl ether. The combined organic layers were washed with a saturated NaHCO3 solution and brine, dried over Na2SO4 and concentrated under reduced pressure. The crude residue was purified by chromatography on silica gel (hexane/EtOAc 10:1) to yield the title compound as a white solid (42.8 mg, 40%).

1. temperatureAfter cooling down to room temperature
2. extractionthe aqueous phase was extracted with diethyl ether
3. washThe combined organic layers were washed with a saturated NaHCO3 solution and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe crude residue was purified by chromatography on silica gel (hexane/EtOAc 10:1)