反应详情

温度

100 °C

To a solution of 4-fluoro aniline (0.412 ml, 4.296 mmol) in acetonitrile (10 ml) potassium carbonate (771 mg, 5.584 mmol) was added followed by addition of 1-benzhydrylazetidin-3-yl methanesulfonate (D19) (1.5 g, 4.72 mmol). The reaction mixture was stirred at 100° C. for 5 minutes under microwave irradiation. Solvents were evaporated under vacuo and the residue was taken in with diethylether (50 ml) then water (50 ml) was added. The aqueous layer was extracted with diethylether (2×30 ml). The organics after solvent evaporation were purified by Biotage SNAP-Si cartridge (25 g) eluting with cyclohexane/ethylacetate from 100-0 to 85/15. Collected fractions, after solvent evaporation afforded the title (D24) (0.5 g)

1. customSolvents were evaporated under vacuo
2. additionwater (50 ml) was added
3. extractionThe aqueous layer was extracted with diethylether (2×30 ml)
4. customThe organics after solvent evaporation
5. customwere purified by Biotage SNAP-Si cartridge (25 g)
6. washeluting with cyclohexane/ethylacetate from 100-0 to 85/15
7. customCollected fractions, after solvent evaporation
8. customafforded the title (D24) (0.5 g)