反应详情

温度

57.5 °C

To the mixture of 8-[(4R,5R)-5-(tert-butyl-dimethyl-silanyloxymethyl)-2,2-dimethyl-[1,3]dioxolan-4-yl methoxy]-10,10-dimethyl-10H-11-oxa-4-aza-benzo[b]fluoren-5-one (Compound GT15-6, 27 mg), MeOH (0.1 ml) and THF (0.3 ml), 0.5 N sulfuric acid (0.1 ml) was added, and the mixture was stirred and heated at 55 to 60° C. for 4 hrs. The reaction mixture was neutralized with saturated aqueous solution of sodium bicarbonate. The resulting solid was filtered and washed with diethyl ether. The filtrate was extracted with the mixture solution of DCM and MeOH (DCM:MeOH=10:1). The organic layer was washed with saturated brine, and dried over magnesium sulfate. The filtered solid and the residues obtained after concentration under reduced pressure were combined and purified by silica gel column (DCM/MeOH) to obtain the title compound (5.4 mg, 28%).

1. additionwas added
2. filtrationThe resulting solid was filtered
3. washwashed with diethyl ether
4. extractionThe filtrate was extracted with the mixture solution of DCM and MeOH (DCM:MeOH=10:1)
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over magnesium sulfate
7. customThe filtered solid and the residues obtained
8. concentrationafter concentration under reduced pressure
9. custompurified by silica gel column (DCM/MeOH)