反应详情

tert-Butyl{2-[4-(3-{3-[(1R)-3-(diisopropylamino)-1-phenylpropyl]-4-hydroxyphenyl}propoxy)phenyl]ethyl}carbamate (Preparation 7, 400 mg, 0.68 mmol) was dissolved in dichloromethane (15 ml) and hydrochloric acid (10 ml of a 2M solution in diethyl ether) was added to the stirred solution at 0° C. After 3 hours the solvent was removed in vacuo, and ethyl acetate (20 ml) and saturated aqueous sodium hydrogen carbonate (10 ml) were added and the organics separated. The aqueous was washed with dichloromethane:methanol (90:10, by volume, 2×20 ml) and the organics combined, dried (magnesium sulphate) and the solvent removed in vacuo. The residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol:880 ammonia (80/20/2.0 by volume) to furnish the title compound as a glass, 135 mg.

1. customAfter 3 hours the solvent was removed in vacuo, and ethyl acetate (20 ml) and saturated aqueous sodium hydrogen carbonate (10 ml)
2. additionwere added
3. washThe aqueous was washed with dichloromethane:methanol (90:10, by volume, 2×20 ml)
4. dry with materialdried (magnesium sulphate)
5. customthe solvent removed in vacuo
6. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane