反应详情

The compound of Example 18A (600 mg, 0.23 mmol) was dissolved in 2.4 mL of dichloromethane, and the resultant solution was cooled to −78° C. (Diethylamino)sulfur trifluoride (DAST, 0.6 mL) was added; the mixture was stirred for 30 minutes, and then quenched by addition of saturated aqueous sodium bicarbonate solution. The mixture was warmed to ambient temperature; the organic phase was dried over Na2SO4. The solvents were removed in vacuo; the residue was purified by chromatography on an Analogix IntelliFlash 280™, eluting with a gradient of 5% to 7% ethyl acetate in hexanes, to give the titled compound, plus some mixed fractions.

1. additionwas added
2. customquenched by addition of saturated aqueous sodium bicarbonate solution
3. dry with materialthe organic phase was dried over Na2SO4
4. customThe solvents were removed in vacuo
5. customthe residue was purified by chromatography on an Analogix IntelliFlash 280™
6. washeluting with a gradient of 5% to 7% ethyl acetate in hexanes