反应详情

温度

125 °C

Methyl 2-(4-(benzo[d]thiazol-6-yl)-6-methyl-2-phenylpyrimidin-5-yl)pentanoate (0.041 g; 0.098 mmol) and lithium iodide (0.039 mg; 0.295 mmol) were placed in a microwave vial and dissolved in pyridine (0.7 mL). The vial was purged with nitrogen and heated to 125° C. for 48 h. The solvent was removed under reduced pressure, the residue was dissolved in water and the pH of the solution was adjusted between 2 and 3 by addition of a solution of hydrochloric acid 6N until a precipitate formed. The precipitate was collected by filtration and dried under reduced pressure over phosphorus pentoxide. Purification by flash-chromatography on silica gel using a gradient of methanol (1-10%) in dichloromethane furnished 0.015 g (35%) of the title compound as a brown solid.

1. customThe vial was purged with nitrogen
2. customThe solvent was removed under reduced pressure
3. dissolutionthe residue was dissolved in water
4. additionthe pH of the solution was adjusted between 2 and 3 by addition of a solution of hydrochloric acid 6N until a precipitate
5. customformed
6. filtrationThe precipitate was collected by filtration
7. dry with materialdried under reduced pressure over phosphorus pentoxide
8. customPurification by flash-chromatography on silica gel using a gradient of methanol (1-10%) in dichloromethane