Hydrochloric Acid → HCID 11185815, compound

Participants

Reaction Steps

1.06 g (0.01 mole) of triethylamine and 0.85 g (0.01 mole) of magnesium chloride were added, at room temperature, to a solution of 0.85 g (0.005 mole) of monopotassium ethyl malonate dissolved in 10 ml of acetonitrile, followed by stirring. Thereto was added 1.1 g (0.005 mole) of 2-phenyl-4-isopropyl-4-methyl-1,3-oxazol-5-one. The mixture was stirred at 60° C. for 8 hours to give rise to a reaction. After the completion of the reaction, the reaction mixture was cooled. Thereto were added 50 ml of water and diluted hydrochloric acid to adjust the mixture to a pH of 4 or less. The mixture was subjected to extraction with ethyl acetate. The organic layer was washed with a saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution, then dried over anhydrous sodium sulfate, and concentrated. The concentrate was subjected to separation by column chromatography to obtain 0.4 g (0.00131 mole) of ethyl 4,5-dimethyl-3-oxo-4-(benzoylamino)hexanoate (yield=26%).

Provenance & Evidence