反应详情

温度

40 °C

A mixture of methyl (1aRS,7bSR)-5-{N-[methoxycarbonyl]-N-[2-(4-chlorobutyryl-amino)-4-fluorobenzenesulfonyl]amino}-1,1a,2,7b-tetrahydrocyclopropa-[c]chromene-4-carboxylate (Intermediate 109, 0.15 g) and dimethylamine (30% aqueous solution, 5 mL) in acetonitrile (10 mL) was stirred and heated at 40° C. for 10 hours. After cooling, the mixture was concentrated under vacuum and the residue was extracted with a mixture of ethyl acetate and THF (50%), dried (Na2SO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by thick layer chromatography on silica, eluting with a mixture of methanol and DCM (10%) to give methyl (1aRS,7bSR)-5-[2-(4-dimethylaminobutyrylamino)-4-fluorobenzenesulfonyl-amino]-1,1a,2,7b-tetrahydrocyclopropa-[c]chromene-4-carboxylate (0.14 g) as a yellow oil.

1. temperatureAfter cooling
2. concentrationthe mixture was concentrated under vacuum
3. extractionthe residue was extracted with a mixture of ethyl acetate and THF (50%)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customThe filtrate was evaporated to dryness
7. customthe residue was purified by thick layer chromatography on silica
8. washeluting with a mixture of methanol and DCM (10%)