反应详情

To sodium hydride (60.0% in oil) (49.0 mg) was added slowly a solution of dimethyl (3,3-dimethyl-2-oxoheptyl)phosphonate (332 mg) in anhydrous tetrahydrofuran (7.30 mL) at 0° C. and the solution was stirred at room temperature for 1 hour. To the reaction solution was added slowly a solution of the compound 5 (336 mg) in anhydrous tetrahydrofuran (2.90 mL) at room temperature and the solution was stirred for 2 hours. To the reaction solution was added 1N hydrochloric acid at 0° C. and the solution was extracted with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous sodium sulfate and concentrated. The obtained residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:2), to give the title compound (211 mg) having the following physical data.

1. stirringthe solution was stirred for 2 hours
2. extractionthe solution was extracted with ethyl acetate
3. washThe organic layer was washed with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customThe obtained residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:2)