反应详情

温度

70 °C

A solution of 1.50 g of 80% m-chloroperbenzoic acid (MCPBA) in 20 mL of 1,2-dichloroethane was added dropwise to a solution of 2.0 g of 3D in 25 mL of 1,2-dichloroethane at room temperature. The resulting mixture was heated at 70° C. for four hours, cooled and extracted with saturated aqueous sodium sulfite solution, until no reaction to starch/iodide paper occurred. The organic phase was separated, washed with saturated aqueous sodium bicarbonate solution, water, brine, dried (Na2SO4) and stripped of solvent. The residue was flash chromatographed over silica gel, with a 2:3 v:v mixture of ethyl acetate and hexane as eluent, to obtain the title compound, as yellow crystals, m.p.: 193°-195° C.

1. temperaturecooled
2. extractionextracted with saturated aqueous sodium sulfite solution, until no reaction to starch/iodide paper
3. customThe organic phase was separated
4. washwashed with saturated aqueous sodium bicarbonate solution, water, brine
5. dry with materialdried (Na2SO4)
6. customchromatographed over silica gel, with a 2:3 v
7. additionv mixture of ethyl acetate and hexane as eluent