反应详情

To a 0° C. mixture of lithium hydride (0.235 g, 29.4 mmol) in tetrahydrofuran and dimethylformamide (30 mL: 10 mL) is added the compound of Example 11 (3.0 g, 7.3 mmol) and the mixture stirred for 0.5 hr. Benzyl bromide (1.257 g, 7.3 mmol) is then added and the reaction stirred 12 hr at room temperature. The reaction is poured into ice-water (100 mL) and the quenched mixture extracted with ethyl acetate (2×100 mL). Concentration gives crude product that is purified by column chromatography on silica gel eluted with ethyl acetate-hexane (1:9) to yield the title compound (2.5 g, 69%). MS m/z 499.0 (M+.1).

1. stirringthe reaction stirred 12 hr at room temperature
2. extractionthe quenched mixture extracted with ethyl acetate (2×100 mL)
3. concentrationConcentration
4. customgives crude product that
5. customis purified by column chromatography on silica gel
6. washeluted with ethyl acetate-hexane (1:9)