反应详情

温度

50 °C

A suspension of Intermediate 3 (5.84 g, 25.09 mmol) and 4-aminophenylsulfur pentafluoride (MANCHESTER, 5.5 g, 25.09 mmol) in ethanol (150 mL) was heated at 50° C. for 1 h. Heating resulted in the precipitation of a solid. The reaction mixture was concentrated under vacuum, redissolved in DCM (300 mL) and washed with aq. Na2CO3 (2×350 mL). The organic layer was dried over Na2SO4 and filtered. Then 8 g of silica gel were added and the mixture was concentrated under vacuum to dryness. The residue was purified (silica gel column, eluting with Hexane/EtOAc mixtures from 100:0 to 50:50%) to afford the title compound as a white solid.

1. temperatureHeating
2. customresulted in the precipitation of a solid
3. concentrationThe reaction mixture was concentrated under vacuum
4. dissolutionredissolved in DCM (300 mL)
5. washwashed with aq. Na2CO3 (2×350 mL)
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. additionThen 8 g of silica gel were added
9. concentrationthe mixture was concentrated under vacuum to dryness
10. customThe residue was purified
11. wash(silica gel column, eluting with Hexane/EtOAc mixtures from 100:0 to 50:50%)