反应详情

A solution of the acid (153) (92 mg, 0.15 mmol) and EDC (38 mg, 0.2 mmol) in dry DCM (2 ml) was stirred at room temperature overnight. Cyclopropylsulfonamide (48 mg, 0.4 mmol) and DBU (76 mg, 0.5 mmol) was added and the mixture was stirred at room temperature for 6 hours. 5% Citric acid was added and the mixture was extracted three times with ethyl acetate. The organic phase was washed with 5% citric acid and brine, dried with sodium sulphate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluted with ether-methanol which gave the title compound (70 mg, 65%), MS (M+H) 720.

1. extractionthe mixture was extracted three times with ethyl acetate
2. washThe organic phase was washed with 5% citric acid and brine
3. dry with materialdried with sodium sulphate
4. customevaporated under reduced pressure
5. customThe residue was purified by column chromatography on silica gel
6. washeluted with ether-methanol which