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以二氯甲烷为溶剂,氯乙酰氯和苯甲醇反应,合成了氯乙酸苄酯。通过红外光谱、紫外光谱和核磁共振氢谱对氯乙酸苄酯结构进行了表征。采用单因素优选法,对反应时间、反应物比例、碱的种类和反应温度等可能影响氯乙酸苄酯收率的因素进行了讨论。结果表明,最适宜的合成条件反应温度为室温,反应时间90 min,n(氯乙酰氯)∶n(苯甲醇)=1.2∶1。氯乙酸苄酯产率为79.4%,高效液相色谱证明氯乙酸苄酯质量分数为98%。
Using dichloromethane as solvent, chloroacetyl chloride and benzyl alcohol reacted to synthesize benzyl chloroacetate. The structure of benzyl chloroacetate was characterized by IR, UV and 1H NMR. The factors affecting the yield of benzyl chloroacetate, such as reaction time, reactant ratio, base type and reaction temperature, were discussed using single factor optimization method. The results showed that the optimum synthesis conditions were as follows: the reaction temperature was room temperature, the reaction time was 90 min, n (chloroacetyl chloride): n (benzyl alcohol) = 1.2:1. The yield of benzyl chloroacetate was 79.4%. The high performance liquid chromatography showed that the mass fraction of benzyl chloroacetate was 98%.