Acetic Acid → HCID 10976084, compound

Participants

Reaction Conditions

Reaction Steps

276 g (2 mole) of 2,3-dimethyl-hydroquinone were suspended in 300 ml of acetic acid and heated to 80° C. with stirring. Through the obtained solution boron trifluoride was bubbled whereby care was taken that the temperature did not exceed 100° C. The reaction mixture was stirred at 120° C. for 3.5 h and then poured into 4 l of ice-water containing 500 g of dissolved sodium acetate. This mixture was stirred for 12 h till the precipitate could be separated by suction. This precipitate was then treated with 3 l of water whereto enough sodium hydrogen carbonate was added to reach a final pH of 7.5. The precipitate was suction filtered again, washed with water till neutral and recrystallized from toluene. Yield: 230 g. Melting point: 151° C. (structure confirmed by NMR).

Provenance & Evidence