反应详情

A solution of the ester (0.21 g, 0.63 mmol, prepared as described in Step A), in 10 ml of CH3CN--H2O(9:1, v/v) was added dropwise to a stirred solution of TEMPO-BF4 in 10 ml CH3CN--H2O (9:1, v/v). Stirring was continued for 2 h and the reaction mixture was concentrated in vacuo. The residue was partitioned between Et2O and H2O. The organic phase was washed with brine and dried (Na2 SO4). Removal of solvent provides a yellow oil which was purified by flash chromatography (silica gel, hexane-EtOAc 2:1) to give 0.18 g of product as an off white solid.

1. concentrationthe reaction mixture was concentrated in vacuo
2. customThe residue was partitioned between Et2O and H2O
3. washThe organic phase was washed with brine
4. customdried (Na2 SO4)
5. customRemoval of solvent
6. customprovides a yellow oil which
7. customwas purified by flash chromatography (silica gel, hexane-EtOAc 2:1)