反应详情

To a well stirred slurry of compound obtained in example 13 (75 mg, 0.2 mmol) and cesium carbonate (73 mg, 0.22 mmol) in dry DMF (5 ml) was added iodomethane (36.92 mg, 0.26 mol) and the mixture was allowed to stir for 1 hr at room temperature under nitrogen atmosphere. The reaction mixture was quenched with ice water (50 ml), and then extracted with ethyl acetate (50 ml). The organic layer was washed with water followed by brine and dried over sodium sulfate. The organic layer was concentrated under vacuum and the crude product was purified by column chromatography to get 40 mg of the pure product (Yields-52%) MP-235.4-240.8° C.

1. customThe reaction mixture was quenched with ice water (50 ml)
2. extractionextracted with ethyl acetate (50 ml)
3. washThe organic layer was washed with water
4. dry with materialdried over sodium sulfate
5. concentrationThe organic layer was concentrated under vacuum
6. customthe crude product was purified by column chromatography