反应详情

To a solution of the compound prepared in Example 363 (0.112 g) in tetrahydrofuran (3 mL) at 0° C. was added a 3.0 M solution of methylmagnesium bromide in diethyl ether (0.27 mL), and the reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was poured onto cold saturated ammonium chloride, and the mixture was extracted with ethyl acetate. The combined organics were washed with brine, dried over magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate:hexanes:triethylamine=80:20:1) to obtain the title compound (0.035 g) having the following physical data.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe combined organics were washed with brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated
5. customThe residue was purified by column chromatography on silica gel (ethyl acetate:hexanes:triethylamine=80:20:1)