可控微波促进非催化无溶剂条件下酚的乙酰/苯甲酰化反应

Microwave-assisted Acetylation and Benzoylation of Phenols under Catalyst-free and Solvent-free Conditions

采用可控微波加热技术,在无溶剂无催化剂的条件下酚类化合物分别与乙酸酐、苯甲酰氯直接酰化反应,“一锅”法高效地合成了系列羧酸苯酯类化合物.考察了酰化试剂的类型、物料比、反应温度、时间对酰化产率的影响,优化出最佳反应条件.当一元酚与乙酸酐的物质的量之比为2∶1.1,微波加热温度为130℃,反应10min,乙酰化产物的产率在92%以上;二元酚发生乙酰化、苯甲酰化反应的时间相对较长,且产物的产率有所降低.在优化实验条件下合成了12种羧酸苯酯,产物结构通过测定熔点、红外光谱进行表征.

Under the condition of catalyst-and solvent-free,controllable microwave heating technology was adopted to accelerate the direct acylation of phenols with acetic anhydride and benzoyl chloride,respectively.The effects of the type of acylation reagent,ratio of reactants,reaction temperature and time on the reaction were investigated.When the ratio of monophenol to acetic anhydride was 2:1.1,microwave heating temperature at 130℃for 10 minutes,the yield of acetylated product was over 92%.The reaction time of acetylation and benzoylation of binary phenol was relatively long,and the yield of the product was slightly reduced.Under the optimized experimental conditions,12 compounds were synthesized by one pot method.The structure of the product was characterized by melting point and infrared spectra.