反应详情

Trifluoroacetic acid (0.5 mL) was added to a mixture composed of di-tert-butyl {2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-7,8-dihydro-2H-6-thia-1,2,3,5-tetraazaacenaphthylen-4-yl}imidodicarbonate of Step 10) of Example 1 (59 mg) and dichloromethane (2 mL) under cooling in an ice bath. Then, the ice bath was removed and the mixture was stirred for two hours. The reaction solution was concentrated under reduced pressure. Then, the resulting residue was dissolved in ethyl acetate and sequentially washed with a saturated sodium bicarbonate solution and brine. The organic layer was dried over anhydrous magnesium sulfate and filtered. Then, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate-methanol) to obtain the title compound (26 mg, 85%) as a solid.

1. temperatureunder cooling in an ice bath
2. customThen, the ice bath was removed
3. concentrationThe reaction solution was concentrated under reduced pressure
4. dissolutionThen, the resulting residue was dissolved in ethyl acetate
5. washsequentially washed with a saturated sodium bicarbonate solution and brine
6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
7. filtrationfiltered
8. concentrationThen, the filtrate was concentrated under reduced pressure
9. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate-methanol)