反应详情

Triethylamine (5.25 mL) and a sulfur trioxide-pyridine complex (2.45 g) were added to a mixture composed of the above 1-(2-amino-4,6-dichloropyrimidin-5-yl)-2-(2,2-dimethyl-[1,3]dioxolan-4-yl)ethan-1-ol (2.32 g) and dimethyl sulfoxide (30 mL) under cooling in an ice bath. The ice bath was removed and the mixture was stirred for two hours. The reaction mixture was added dropwise to a 0.5 N hydrochloric acid solution (300 mL), followed by extraction with ethyl acetate. The organic layer was sequentially washed with water and brine and then dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure and the solvent was evaporated to obtain a crude product of the title compound (2.08 g, 90%) as a solid. The resulting compound was directly used for the next reaction without purification.

1. temperatureunder cooling in an ice bath
2. customThe ice bath was removed
3. additionThe reaction mixture was added dropwise to a 0.5 N hydrochloric acid solution (300 mL)
4. extractionfollowed by extraction with ethyl acetate
5. washThe organic layer was sequentially washed with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationAfter filtration
8. concentrationthe filtrate was concentrated under reduced pressure
9. customthe solvent was evaporated