Synthesis of Intermediate N-Chloroformyl-N-[4-(trifluoromethoxy)phenyl]Methyl Carbamate of Indoxacarb

[Objective]The paper was to study a synthetic method suitable for industrial production of intermediate N-Chloroformyl-N-[4-(trifluoromethoxy)phenyl]methyl carbamate of indoxacarb.[Method]Using 4-trifluoromethoxy aniline as the starting material,[4-(trifluoromethoxy)phenyl]carbamate was synthesized by homogeneous formylation method without acid-binding agent.Subsequently,it was reacted with sodium methoxide/potassium methoxide by reactive distillation to obtain[4-(trifluoromethoxy)phenyl]carbamate ammonium sodium/potassium,then directly reacted with triphosgene to obtain crude products of N-carbonochloridoyl-N-[4-(trifluoromethoxy)phenyl]carbamate;finally,competing product was obtained by recrystallization.[Result]The intermediate N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]carbamate was synthesized by the method.The content of products was higher than 98%.The yield of product reached above 96%(calculated by 4-trifluoromethoxy aniline).[Conclusion]The method used for the synthesis of intermediate N-chloroformyl-N-[4-(trifluoromethoxy)phenyl]methyl carbamate was simple,with less three wastes,higher safety and lower cost.

杀虫剂Flometoquin的合成与生物活性研究

以4-三氟甲氧基苯酚和2-甲基-4-硝基氯苯为初始原料制备了Flometoquin,其结构经1H NMR和LC-MS表征确证。生物活性研究表明其对同翅目害虫的蚜虫具有卓越的杀虫活性,在50 mg/L浓度下活性达90%;对螨红蜘蛛活性不明显,在500 mg/L浓度下活性不足50%。

对三氟甲氧基苯胺合成催化剂失活研究

采用固定床反应器考察自制Pt/C催化剂催化对三氟甲氧基硝基苯加氢合成对三氟甲氧基苯胺反应性能,并用ICP、N 2吸附、SEM、TEM和EDS对加氢失活催化剂进行表征分析。结果表明,催化加氢过程F离子及积碳在催化剂表面金属活性位上吸附覆盖是造成催化剂活性降低的主要原因,失活催化剂再生后表面F离子和积碳去除,孔结构和催化加氢活性恢复。