以苯甲醛为原料,与磷酰基乙酸三乙酯在氢化钠存在下反应制备肉桂酸乙酯,后通过水解制备肉桂酸,总收率95%。考察了温度、溶剂、反应时间、物料摩尔比对肉桂酸乙酯收率的影响。结果表明,最佳反应条件为室温下,以二氯甲烷为溶剂,反应2 h,苯甲醛、磷酰基乙酸三乙酯、氢化钠摩尔比为1:1.5:1.5,该步反应收率97%,水解反应收率98%。利用该优化方案合成了一系列肉桂酸衍生物,收率均在92%以上,结构通过质谱、核磁鉴定正确。%Using benzaIdehyde as starting materiaI,ethyI cinnamate was synthesized with triethyI phospho-noacetate in the presence of sodium hydride. Cinnamic acid was prepared through hydroIysis of the ester in 95% totaI yieId. YieId of ethyI cinnamate as an index,the reaction conditions such as temperature,soI-vent,time,reactant ratio were studied. ResuIt showed that the optimum reaction condition was as foIIows:At room temperature,with dichIoromethane as soIvent,reaction 2 h,benzaIdehyde,triethyI phosphonoace-tate and sodium hydride moIe ratio of 1 :1 . 5 :1 . 5 was the best conditions to generate ethyI cinnamate with 97% yieId. The hydroIysis yieId was 98%. With over 92% totaI yieIds,a series of cinnamic acid de-rivatives were synthesized by using this method. Structure was characterized by mass spectrometry and nu-cIear magnetic.
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