反应详情

To 0.64 g (1.42 mmol) of 4 dissolved in 10 mL of THF was added 0.177 mL (2.85 mmol) of iodomethane followed by 0.11 g (2.8 mmol) of sodium hydride (60% dispersion in mineral oil). After stirring at room temperature for 2 h, the reaction was quenched by addition of approximately 2 mL of saturated aqueous ammonium chloride. The reaction was then diluted with AcOEt and dried over sodium sulfate. Filtering the solution through a short plug of silica gel and concentrating in vacuo provided the crude product. Purification by flash chromatography eluting with 90% hexanes/ethyl acetate gave 0.42 g (64%) of the title compound as a cream colored powder. MS Calcd.: 463. Found: 464 (M+H).

1. customthe reaction was quenched by addition of approximately 2 mL of saturated aqueous ammonium chloride
2. additionThe reaction was then diluted with AcOEt
3. dry with materialdried over sodium sulfate
4. filtrationFiltering the solution through a short plug of silica gel
5. concentrationconcentrating in vacuo
6. customprovided the crude product
7. customPurification by flash chromatography
8. washeluting with 90% hexanes/ethyl acetate