反应详情

tert-Butyl (3S,5R)-3-[({4-[(3-methoxypropyl)amino]-6-(1-methylethyl)pyridin-3-yl}carbonyl)(2-methylpropyl)amino]-5-(morpholin-4-ylcarbonyl)piperidine-1-carboxylate (268 mg) was dissolved in 4 M hydrogen chloride-ethyl acetate (5 ml), and the mixture was stirred at room temperature for 15 hr. The reaction mixture was concentrated, the residue was purified by reversed-phase preparative HPLC, and the object fraction was concentrated under reduced pressure. Aqueous sodium hydrogen carbonate was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. 4 M Hydrogen chloride-ethyl acetate (1 ml) was added to the residue, and the mixture was stirred for 5 min and concentrated under reduced pressure to give the object compound (163 mg).

1. concentrationThe reaction mixture was concentrated
2. customthe residue was purified by reversed-phase preparative HPLC
3. concentrationthe object fraction was concentrated under reduced pressure
4. additionAqueous sodium hydrogen carbonate was added to the residue
5. extractionthe mixture was extracted with ethyl acetate
6. washThe extract was washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. addition4 M Hydrogen chloride-ethyl acetate (1 ml) was added to the residue
10. stirringthe mixture was stirred for 5 min
11. concentrationconcentrated under reduced pressure