Kong Xian-ming
2006
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Journal
Fine chemicals
Abstract
2-Hydroxy-4-methoxybenzophenone(UV-9) was synthesized from 2,4-dihydroxybenzo-phenone and dimethyl sulfate.The polarity of solvent has great influence on the reaction.Solvents of too high or too low polarity can′t be used.Acetone is suitable for this reaction because of its moderate polarity.Phase transfer catalyst has no effect on the reaction.Thus,reflux 0.2 mole 2,4-dihydroxybenzophenone and 0.2 mole dimethyl sulfate in 40 mL acetone with 0.12 mole potassium carbonate for 4.0 h,remove the acetone after the reaction,wash the crude product with hot water,and recrystallize the product in ethanol.The isolated yield of UV-9 was up to 87%.Industrial synthesis was carried out in 3 m~3 reactor with feedstock of 910 kg acetone,322 kg K_2CO_3,830 kg 2,4-dihydroxybenzophenone and 489 kg dimethyl sulfate by the same procedure and the yield of UV-9 reached 89%.The recovered acetone was reused ten times and the yield of UV-9 can still attain 88%.