反应详情

Stir a solution of 4-[2-(4-methanesulfonyl-phenyl)-6-methoxy-naphthalen-1-yloxy]-phenol (160 mg, 0.39 mmol), 2-(hexamethyleneimino)-ethyl chloride hydrochloride (140 mg, 0.69 mmol), 60% sodium hydride (47 mg, 1.18 mmol) and N,N-dimethylformamide (2 mL) for 18 hours at ambient temperature, then evaporate under reduced pressure. Dissolve the residue in dichloromethane and wash with water, dry with solid magnesium sulfate and chromatograph on silica gel with dichloromethane/methanol mixtures. Combine the fractions containing product and add 1N hydrogen chloride in diethyl ether (0.30 mL). Concentrate the resulting solution under reduced pressure to give 160 mg of the title compound (69%). Mass spectrum (ion spray): m/z=546 (M+H).

1. customevaporate under reduced pressure
2. dissolutionDissolve the residue in dichloromethane
3. washwash with water
4. dry with materialdry with solid magnesium sulfate and chromatograph on silica gel with dichloromethane/methanol mixtures
5. additionCombine the fractions containing product
6. additionadd 1N hydrogen chloride in diethyl ether (0.30 mL)
7. concentrationConcentrate the resulting solution under reduced pressure