反应详情

A mixture of methyl (1aRS,7bSR)-5-amino-1,1a,2,7b-tetrahydrocyclopropa-[c]chromene-4-carboxylate (Intermediate 42, 0.1 g), 4-fluoro-2-nitrobenzenesulfonyl chloride (0.115 g) and pyridine (2 mL) in DCM (5 mL) was stirred at room temperature overnight. The mixture was concentrated under vacuum and the residue was partitioned between ethyl acetate and water. The organic layer was dried (Na2SO4) and filtered and the filtrate was evaporated to dryness. The residue was purified by chromatography on silica, eluting with a mixture of ethyl acetate and petroleum ether (20%) to give methyl (1aRS,7bSR)-5-(4-fluoro-2-nitrobenzenesulfonylamino)-1,1a,2,7b-tetrahydrocyclopropa[c]chromene-4-carboxylate (0.11 g) as a yellow oil.

1. concentrationThe mixture was concentrated under vacuum
2. customthe residue was partitioned between ethyl acetate and water
3. dry with materialThe organic layer was dried (Na2SO4)
4. filtrationfiltered
5. customthe filtrate was evaporated to dryness
6. customThe residue was purified by chromatography on silica
7. washeluting with a mixture of ethyl acetate and petroleum ether (20%)