反应详情

The crude compound (7R)-2-chloro-7-ethyl-8-isopropyl-5,7-dihydropteridin-6-one 22c (12.10 g, 47.50 mmol) was dissolved in 180 mL of acetone followed by the addition of methyl p-toluenesulfonate (13.28 g, 71.30 mmol) and potassium carbonate (13.11 g, 95 mmol). The reaction solution was heated to reflux for 3 hours with stirring and filtered. The filtrate was concentrated under reduced pressure, added with 100 mL of water and extracted with dichloromethane (100 mL×3). The combined organic phase was washed with saturated sodium chloride solution (100 mL), then dried over anhydrous magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (7R)-2-chloro-7-ethyl-8-isopropyl-5-methyl-7H-pteridin-6-one 22d (10.80 g, yield: 84.7%) as a white solid.

1. temperatureThe reaction solution was heated
2. temperatureto reflux for 3 hours
3. filtrationfiltered
4. concentrationThe filtrate was concentrated under reduced pressure
5. additionadded with 100 mL of water
6. extractionextracted with dichloromethane (100 mL×3)
7. washThe combined organic phase was washed with saturated sodium chloride solution (100 mL)
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationfiltered
10. concentrationthe filtrate was concentrated under reduced pressure
11. customThe resulting residue was purified by silica gel column chromatography