反应详情

Methanesulfonic anhydride (1.24 g, 7.13 mmol) was added to a solution of the product of Example 11, Step C (1.3 g, 3.86 mmol) and triethylamine (1.17 g, 11.6 mmol) in anhydrous THF (50 mL) at ambient temperature. After stirring for 1 h, morpholine (3 mL) was added and the reaction mixture was heated at reflux temperature for 1 h followed by removal of solvent. A saturated aqueous solution of sodium bicarbonate was added and the mixture was extracted with ethyl acetate (2×100 mL). The combined extracts were dried (MgSO4) and evaporated to an oil which was purified by column chromatography (silica, 30% to 60% ethyl acetate/hexane) to give a solid (1.39 g, 88%): mp 112°-114° C.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux temperature for 1 h
3. customfollowed by removal of solvent
4. additionA saturated aqueous solution of sodium bicarbonate was added
5. extractionthe mixture was extracted with ethyl acetate (2×100 mL)
6. dry with materialThe combined extracts were dried (MgSO4)
7. customevaporated to an oil which
8. customwas purified by column chromatography (silica, 30% to 60% ethyl acetate/hexane)