反应详情

To a solution of the product from Step A (0.95 g, 3.19 mmol) in DMF (10 mL) was added cesium carbonate (1.26 g, 3.70 mmol) followed by iodomethane (0.23 mL, 3.70 mmol) at room temperature. After stirring for 3 h, saturated aqueous ammonium chloride (30 mL) was added and the mixture extracted with ethyl acetate (3×65 mL). The combined extracts were washed with brine (10 mL), dried (MgSO4) and evaporated to a residue which was purified by chromatography (silica, 20% ethyl acetate in hexane to 30% ethyl acetate in hexane) to give a syrup (0.63 g, 92%): MS (ES) m/z 340(M+).

1. extractionthe mixture extracted with ethyl acetate (3×65 mL)
2. washThe combined extracts were washed with brine (10 mL)
3. dry with materialdried (MgSO4)
4. customevaporated to a residue which
5. customwas purified by chromatography (silica, 20% ethyl acetate in hexane to 30% ethyl acetate in hexane)