甲基 4-氧代-4-苯基丁-2-烯酸乙酯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.90 g of methyl 3-benzoylacrylate was dissolved in 30 ml of diethyl ether, and 0.8 ml of thioacetic acid was added thereto. The mixture was stirred for 5 hours at room temperature. The reaction solution was washed, in turn, with water, a saturated aqueous solution of sodium hydrogencarbonate and water, and dried over magnesium sulfate. The diethyl ether was removed from the solution by evaporation, and the residue was purified by silica gel column chromatography using a mixture of hexane and diethyl ether as an eluent, and then recrystallized from the same mixture to give 2.42 g of methyl 2-acetylthio-3-benzoylpropionate. The reaction solution was washed, in turn, with water a saturated aqueous solution of sodium hydrogencarbonate and water, and dried over magnesium sulfate The diethyl ether was removed from the solution by evaporation the residue was purified by silica gel column chromatography a mixture of hexane and diethyl ether as an eluent recrystallized from the same mixture