反应详情

Methyl 3-(1-tert-butoxycarbonylpiperidin-3-yloxy)-12-cyclohexyl-6,7-dihydro-5-oxa-7a-azadibenzo[a,e]azulene-9-carboxylate (0.68 g) was dissolved in trifluoroacetic acid (20 ml), and the mixture was stirred at room temperature for 3 hr. Toluene was added to the reaction mixture and the solvent was evaporated under reduced pressure. 4N HCl-ethyl acetate solution (2.0 ml) was added to the obtained residue and the mixture was stirred, and the solvent was evaporated under reduced pressure. The residue was neutralized with saturated aqueous sodium hydrogen carbonate solution and extracted with ethyl acetate. The organic layer was successively washed with water and saturated brine and dried over anhydrous magnesium sulfate. After filtration, the solvent was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (chloroform:methanol=9:1) to give methyl 12-cyclohexyl-3-(piperidin-3-yloxy)-6,7-dihydro-5-oxa-7a-azadibenzo[a,e]azulene-9-carboxylate (0.16 g, yield 17%).

1. customthe solvent was evaporated under reduced pressure
2. addition4N HCl-ethyl acetate solution (2.0 ml) was added to the obtained residue
3. stirringthe mixture was stirred
4. customthe solvent was evaporated under reduced pressure
5. extractionextracted with ethyl acetate
6. washThe organic layer was successively washed with water and saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationAfter filtration
9. concentrationthe solvent was concentrated under reduced pressure
10. customthe residue was purified by silica gel chromatography (chloroform:methanol=9:1)