反应详情

3-Chloroperoxybenzoic acid (7.8 g of 77%) was added in a single portion to a solution of tert-butyl N-{4-[2-(2-methoxyethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]butyl}carbamate (7 g) in dichloroethane (100 mL). The reaction mixture was stirred at ambient temperature for 3 hours, Concentrated ammonium hydroxide (100 mL) was added and the reaction mixture was stirred until a suspension formed. Para-toluenesulfonyl chloride (3.6 g) was added in a single portion. The reaction mixture was stirred at ambient temperature for 2 hours and then diluted with dichloromethane and brine. The organic layer was separated, washed with brine (×2), dried over magnesium sulfate, filtered through a layer of CELITE filter aid, and then concentrated under reduced pressure to provide 8.83 g of crude tert-butyl N-{4-[4-amino-2-(2-methoxyethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]butyl}carbamate as a brown solid.

1. stirringthe reaction mixture was stirred until a suspension
2. customformed
3. stirringThe reaction mixture was stirred at ambient temperature for 2 hours
4. customThe organic layer was separated
5. washwashed with brine (×2)
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered through a layer of CELITE
8. filtrationfilter aid
9. concentrationconcentrated under reduced pressure