反应详情

To a stirred solution of Compound B (150 mg, 0.6 mmol) in methylene chloride with saturated NaHCO3 solution was added 4-fluorobenzenesulfonyl chloride (300 mg, 1.55 mmol). The mixture was stirred at room temperature for 18 h and diluted with methanol. 10 N NaOH was added and the mixture was stirred for 2 h. Concentrated NH4OH was added and the mixture was stirred for 18 h and concentrated in vacuo. The residue was partitioned between ethyl acetate and saturated NaHCO3. The organic layer was separated, dried over MgSO4, and concentrated in vacuo. The residue was purified by chromatography (1:4, ethyl acetate and hexanes) to give Compound C as an oil (120 mg, 50%).

1. stirringthe mixture was stirred for 2 h
2. stirringthe mixture was stirred for 18 h
3. concentrationconcentrated in vacuo
4. customThe residue was partitioned between ethyl acetate and saturated NaHCO3
5. customThe organic layer was separated
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customThe residue was purified by chromatography (1:4, ethyl acetate and hexanes)