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作 者:刘焕梅[1] 李立军[2] 孙晓然[3] 韩美慧[4] 刘焕昱
机构地区:[1]河北联合大学轻工学院 [2]河北大学化学与环境科学学院,河北保定071002 [3]河北联合大学化学工程学院 [4]湘南学院临床医学系,10级8班湖南郴州023000 [5]沧州市市政工程公司,河北沧州061000
出 处:《化学世界》2013年第10期608-611,共4页Chemical World
摘 要:改进2,4-二氯苯氧乙酸(2,4-D)传统的合成工艺。主要反应不是采取先氯化的方法,而是先以苯酚和氯乙酸缩合后,再用次氯酸钠进行氯化的后氯化法,进而用正交试验,确定了新方法的最佳工艺条件:投料比为苯氧乙酸/g∶冰醋酸/mL=1∶9,次氯酸钠投入量为18mL(滴加),反应温度为冰水浴中进行,酸化至pH<1条件下,产品收率最高。测定了产品的mp IR和NMR,均与文献值相符。The synthesis method of 2,4-dichlorophenoxyacetic acid (2,4-D) was improved. In the first step chloroacetic acid and phenol were used as raw materials, After that sodium hypochlorite (NaC10) was used as chloration agent. The optimum reaction conditions were obtained by orthogonal experiments. When the ratio of phenoxyacetic acid/g: glacial acetic acid/mL was 1 : 9, 18 mL of sodium hypochlorite was added dropwise the reaction was carried out in ice water bath, and the pH . 1, the product yield was the highest. The results of rap, IR and i H NMR of the product agreed with those in the literature.
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