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正交设计法优化3-氯-2,4-二氟溴苯合成工艺
作者姓名:宗建成  刘峰  蒋涛
作者单位:常州刘国钧高等职业技术学校,江苏常州,213025;常州工程职业技术学院化学工程技术系,江苏常州,213164
摘    要:以2, 6-二氟氯苯为原料,经过N-溴代丁二酰亚胺(NBS)溴代反应生成3-氯-2,4-二氟溴苯。以收率为评价指标,进行了L16(44)正交试验,考察了原料配比、反应温度、反应时间对收率的影响,获得了最佳反应条件:2, 6-二氟氯苯与NBS物质的量比为1∶1.09、2,6-二氟氯苯与浓硫酸物质的量比为1∶15,反应温度为0℃,反应时间为4 h。最佳反应条件验证实验显示,产品收率高达90%。

关 键 词:3-氯-2    4-二氟溴苯  2    6-二氟氯苯  溴代反应  正交实验

Optimization of the synthesis process of 1-bromo-3-chloro-2,4-difluorobenzene by the orthogonal design method
Authors:Zong Jiancheng  Liu Feng  Jiang Tao
Affiliation:(Changzhou Liuguojun Vocational Technology College,Changzhou 213025,China;department of Chemical Engineering,Changzhou Institute of Engineering Technology,Changzhou 213164,China)
Abstract:1-Bromo-3-chloro-2, 4-difluorobenzene was synthesized by using 1-chloro-2, 6-difluorobenzene and n-bronusuccinimide(NBS) as raw materials through the bromine reaction. The mole ratio of the materials, the reaction temperature and reaction time were investigated by the single factor experiment,with the yield of the product as index,the best reaction condition was studied through orthogonal test of L16(44).The optimum reaction conditions is the mole ratio of 1-chloro-2, 6-difluorobenzene to is 1∶1.09, the molar ratio of 1-chloro-2, 6-difluorobenzene to sulfuric acid is 1∶15,the reaction temperature was 0℃ and the reaction time is 4.0 h. Under the optimum synthetic conditions, the yield of the product is up to 90%.
Keywords:1-bromo-3-chloro-2  4-difluorobenzene  2  6-difluorobenzene  bromine reaction  orthogonal experime
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