反应详情

温度

35 °C

A solution of 13.8 g of MCPBA in 100 ml of methylene chloride was added drop-by-drop over 10 minutes to a stirred solution of 16.1 g of 1G in 150 ml of methylene chloride at room temperature. The resulting mixture was stirred and refluxed (35° C.) for 30 minutes, then washed with 10% aqueous sodium carbonate solution. The resulting methylene chloride solution was dried (MgSO4), and the solvent was evaporated. The residue was purified by column chromatography over silica gel, using a 1:4:20 v:v:v mixture of THF, ethyl acetate and hexane as eluent, to give 1, as a brick red solid, m.p.: 95°-97° C.

1. washwashed with 10% aqueous sodium carbonate solution
2. dry with materialThe resulting methylene chloride solution was dried (MgSO4)
3. customthe solvent was evaporated
4. customThe residue was purified by column chromatography over silica gel
5. additionv:v mixture of THF, ethyl acetate and hexane as eluent
6. customto give 1