反应详情

温度

37 °C

A solution of 5.3 g of 85% m-chloroperoxybenzoic acid (MCPBA) in 100 ml of methylene chloride was added slowly to a solution of 6.2 g of 1F in 100 ml of methylene chloride, at room temperature. The mixture warmed to about 37° C. It was allowed to cool to room temperature, let stand for 18 hours, washed with 10% aqueous sodium carbonate solution, then water, then the liquid phases were separated. The methylene chloride phase was dried (MgSO4) and the solvent was evaporated. The residue was crystallized from ether/hexane (1:1, v:v) to give 1, as an orange solid, m.p.: 62°-65° C.

1. temperatureto cool to room temperature
2. washwashed with 10% aqueous sodium carbonate solution
3. customwater, then the liquid phases were separated
4. dry with materialThe methylene chloride phase was dried (MgSO4)
5. customthe solvent was evaporated
6. customThe residue was crystallized from ether/hexane (1:1, v:v)
7. customto give 1