反应详情

To a solution of the product from Step C (1.60 g, 4.75 mmol) and triethylamine (1.44 g, 14.2 mmol) in anhydrous THF (100 mL) at ambient temperature was added methanesulfonic anhydride (1.24 g, 7.13 mmol). After 1 h, the reaction mixture was divided into two equal portions; to one of these portions was added bis(2-methoxyethyl)amine (6 mL). The mixture was stirred for 72 h, evaporated to dryness and the residue extracted with ethyl acetate (2×100 mL). The combined extracts were dried (MgSO4), filtered and evaporated to a residue which was purified by column chromatography (silica, 20-30% ethyl acetate/hexane) to give an oil (0.71 g) which solidified upon standing: mp 75°-77° C.

1. customevaporated to dryness
2. extractionthe residue extracted with ethyl acetate (2×100 mL)
3. dry with materialThe combined extracts were dried (MgSO4)
4. filtrationfiltered
5. customevaporated to a residue which
6. customwas purified by column chromatography (silica, 20-30% ethyl acetate/hexane)