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2,6-二氟苯腈的合成
Synthesis of 2,6-Difluorobenzonitrile
【摘要】 以2,6二氯苯腈(DCBN)和氟化钾为原料,采用非极性溶剂环丁砜为反应介质,经氟化合成了2,6二氟苯腈(DFBN)。对影响产率的诸因素进行了考察,其最佳工艺条件是:n (DCBN)∶n(KF)∶n(季铵盐)∶n(阻聚剂)=1∶2-6∶0-02∶0-04,反应温度为170~175 ℃( 第一步)和220 ℃(第二步) ,反应时间为1-5 h(第一步)和3-5 h(第二步),产品的收率可达90% 左右,纯度≥98% 。
【Abstract】 Difluorobenzonitrile(DFBN) was prepared by 2,6 dichlorobenzonitrile(DCBN) and KF using sulfolane as a non polar solvent.Factors influencing the yield were discussed.The optimum reaction conditions were as follow: n(DCBN)∶ n(KF)∶ n(quaternaries)∶ n(inhibitor) = 1∶2 6∶0 02∶0 04 ,reaction temperature 170~175 ℃(in the first step) and 230 ℃ (in the second step) and reaction time 1 5 h (in the first step) and 3 5 h (in the second step). The yield of the product reached 90% and the purity was 98%.
【Key words】 difluorobenzonitrile; 2,6 dichlorobenzonitrile; potassium fluoride; fluorination;
- 【文献出处】 精细化工 ,FINE CHEMICALS , 编辑部邮箱 ,2000年01期
- 【分类号】TQ242.1
- 【被引频次】5
- 【下载频次】315