反应详情

Di-tert-butyl{9-[4-({3-[(R)-cyclohexyl(hydroxy)phenylmethyl]-1H-1,2,4-triazol-1-yl}methyl)piperdin-1-yl]nonyl}imidodicarbonate (Preparation 5, 2.6 g, 3.7 mmol) was dissolved in dichloromethane (15 ml) and hydrogen chloride in diethylether (2M, 15 ml, 30 mmol) added. After stirring at room temperature for 5 hours the solvent was removed in vacuo, the residue was partitioned between dichloromethane (200 ml) and saturated aqueous sodium bicarbonate solution (200 ml). The organic layer was separated, dried over magnesium sulphate, filtered and the solvent removed in vacuo. The residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol:880 ammonia (97.5:2.5:0.25, by volume) to furnish the title compound as a clear oil, in 70% yield, 1.29 g (contains 10% of other triazole regio-isomer).

1. customwas removed in vacuo
2. customthe residue was partitioned between dichloromethane (200 ml) and saturated aqueous sodium bicarbonate solution (200 ml)
3. customThe organic layer was separated
4. dry with materialdried over magnesium sulphate
5. filtrationfiltered
6. customthe solvent removed in vacuo
7. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane