反应详情

4-{4-[(6-Aminohexyl)oxy]butyl}-2-[(1R)-3-(diisopropylamino)-1-phenylpropyl]phenol (Preparation 26, 153 mg, 0.32 mmol) and N-{2-(benzyloxy)-5-[(1R)-2-bromo-1-{[tert-butyl(dimethyl)silyl]oxy}ethyl]phenyl}methanesulfonamide (Prepared according to WO2005/080324, 155 mg, 0.32 mmol), potassium iodide (10 mg) and sodium hydrogen carbonate (104 mg, 1.23 mmol) were heated in propionitrile (3 ml) at 90° C. for 24 hours. The reaction was cooled to room temperature and the solvent removed in vacuo. The residue was dissolved in ethyl acetate (30 ml), washed with aqueous saturated sodium hydrogen carbonate (30 ml), water (30 ml), brine (30 ml) and dried (magnesium sulphate). The solvent was removed in vacuo and the oil was purified by column chromatography on silica gel eluting with dichloromethane:methanol:880 ammonia (8511511.5 by volume) to furnish the title compound as a yellow oil, 130 mg.

1. customthe solvent removed in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate (30 ml)
3. washwashed with aqueous saturated sodium hydrogen carbonate (30 ml), water (30 ml), brine (30 ml)
4. dry with materialdried (magnesium sulphate)
5. customThe solvent was removed in vacuo
6. customthe oil was purified by column chromatography on silica gel eluting with dichloromethane