反应详情

PPh3 (2.0 eq.) and C2Cl6 (2.0 eq.) were dissolved in DCM (0.72 M) at room temperature and Et3N (4.0 eq.) was added, followed after 5 min of stirring by dropwise addition of a solution of F3 in DCM (0.36 M). The mixture was stirred at room temperature for 1 h and then was diluted with DCM, washed with brine, dried (Na2SO4), filtered and concentrated under reduced pressure. Crude was purified by column chromatography (eluent: Petroleum ether/EtOAc from 94:6 to 2:3) to give the title compound as orange oil. MS (ES+) C32H37N3O6: 560 (M+H)+.

1. washwashed with brine
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customCrude was purified by column chromatography (eluent: Petroleum ether/EtOAc from 94:6 to 2:3)