4-甲氧基二苯甲酰基甲烷的合成研究

Study on synthesis of 4-methoxydibenzonylmethane

以苯甲醛、4 甲氧基苯乙酮为原料,经缩合,加成,成环,水解四步反应合成了4 甲氧基二苯甲酰基甲烷.较系统地研究了反应温度,反应时间,催化剂用量对产品收率的影响.实验表明:苯亚甲基4 甲氧基苯乙酮(Ⅰ)用甲醇作溶剂,NaOH(ωNaOH=10%)作催化剂,反应温度50～55℃,反应时间50min时收率可达92%.4 甲氧基二苯甲酰基甲烷(Ⅱ)用二甲苯作溶剂,0.08mol的CH3ONa/CH3OH(ωCH3ONa/CH3OH=30.0%)和HCl(ωHCl=37.0%)作催化剂,加成,成环,水解反应时间为1h,1h,2h;反应温度为48～50℃,80℃,80℃时收率达58%.产品总收率为53.4%.

4-methoxydibenzonylmethane was synthesized from benzaldehyde and 4-methoxyacetophenone through a series of reactions of condensation, addition, cyclization and hydrolysis. The factors influencing (the synthesis) were discussed and the best conditions were found out. The optimum conditions of (benzylidene-4-methoxyacetophenone) (Ⅰ) synthesized are that the catalyst was 100ml NaOH (ω_(NaOH)=10%), the reaction temperature reached 50℃～55℃, the reaction time was 50 min, and the yield of (Ⅰ) was 92%. And 4-methoxydibenzonylmethane (Ⅱ) synthesized are that the catalyst was 0.08 mol CH_3ONa/CH_3OH(ω_(CH_3Na/CH_3OH)=30.0%) and 0.08 mol HCl(ω_(HCl)=37.0%), the reaction time of was an hour and the reaction temperature was 48～50℃ in addition; the reaction time was an hour and the reaction temperature was 80℃ in cyclization; the reaction time was two hours and the reaction temperature was 80℃ in hydrolysis; and the yield of (Ⅱ) was 58%. The total yield of 4-methoxydibenzonylmethane can reach 53.4%.