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在超声波促进下以磷酸为催化剂,乙酸酐为酰化剂对二茂铁专一性酰化反应得到了高产率的乙酰二茂铁。探讨了超声波设置温度和时间、反应物摩尔比、催化剂用量以及投料方式对反应产率的影响。结果表明:二茂铁、乙酸酐和磷酸的摩尔比为1:16:5,超声波温度为60℃下反应15min,产率可达91.3%。反应产物经薄层色谱、高效液相色谱、熔点测定以及红外光谱表征。
Activated by ultrasonic wave, phosphoric acid was used as the catalyst, acetic anhydride as the acylating agent, and ferrocene-specific acylation reaction gave high yield of acetylferrocene. The effects of ultrasonic setting temperature and time, molar ratio of reactants, catalyst dosage and feeding mode on the reaction yield were discussed. The results showed that the molar ratio of ferrocene, acetic anhydride and phosphoric acid was 1: 16: 5, the reaction temperature was 60 ℃, reaction time was 15min, the yield was 91.3%. The reaction product was characterized by thin layer chromatography, high performance liquid chromatography, melting point determination and infrared spectroscopy.