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作 者:陆阳[1] 徐固华[2] 董超宇[3] 陶京朝[1] 张志荣[4] 冯世龙[2]
机构地区:[1]郑州大学化学系,河南郑州450001 [2]信阳农业高等专科学校有机化学教研室,河南信阳464000 [3]开封大学化工系,河南开封475000 [4]安徽省华祥农药化工公司,安徽合肥230041
出 处:《应用化工》2006年第1期54-56,59,共4页Applied Chemical Industry
摘 要:以2,4-二氟硝基苯和2,6-二氯苯腈为起始原料,经过6步反应合成伏虫隆,总收率为75.3%。以2,4-二氟硝基苯为原料,经过氯化、还原反应合成3,5-二氯-2,4-二氟苯胺(I),产率为84.5%;以2,6-二氯苯腈为原料,经过氟化和水解,制得2,6-二氟苯甲酰胺(Ⅱ),产率为87.7%;将Ⅱ与二(三氯甲基)碳酸酯(BTC)酰化,合成2,6-二氟苯甲酰异氰酸酯(Ⅲ),产率为91.3%;Ⅲ与Ⅰ加成,得到杀虫剂伏虫隆,产率为95%。产物结构经元素分析、IR和1H NMR表征。该工艺具有原料易得、收率高、质量好、对环境污染小等特点。Teflubenzuron was synthesized h, om 2,4-difluoronitrobenzene and 2,6-dichlobenil as starting reagent through six-step reaction with the yield of 75.3%. 3,5-Dichloro-2,4-difluoroaniline( Ⅰ ) was synthesized by chlorination ,reduction reaction from 2,4-difluoronitrobenzene, the yield was 84.5% ;2,6-difluoro- benzamide( Ⅱ ) with the yield of 87.7% was synthesized by fluoridation and hydrolysis from 2,6-dichlobenil. An acylation reaction of Ⅱ and bis (trichloro-methyl) carbonate produced 2,6-difluorobenzoly isocyanate(Ⅲ) ,the yield was 91.3% ;followed by reacting with Ⅲ and Ⅰ to synthesize insecticide teflubenzuron, the yield was 95%. The product structure was characterized by elemental analyses, IR spectra and ^1HNMR. It has characteristics of ready availability of reactant, high yield, good quality, little pollution to environment.
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