文档介绍:摘要本论文是关于菊酯类农药七氟菊酯的合成和工艺优化的研究,重点优化了重要中间体四氟对甲基苄醇的合成工艺,并对目标产物七氟菊酯的合成路线进行了改进。以四氯对苯二甲酸为原料,经酰氯化、氟化、酯化、还原、溴化、还原六步反应合成了四氟对甲基苄醇。四氟对甲基苄醇再经氯化、与(z).ORS,3RS).3.(2-氯·3,3,3-三氟丙-l一丙烯基)一2,(功夫酸)酯化合成了七氟菊酯。重点对工艺路线中溴化、还原反应进行了优化。以甲苯为溶剂,四氟对苯二苄醇与氢溴酸反应制得四氟对溴甲基苄醇,将氢溴酸的用量从四氟对苯二苄醇的摩尔量10倍降低至5倍,%%。四氟对溴甲基苄醇被镁粉和甲醇还原生成四氟对甲基苄醇,通过采用替代溶剂,将镁粉的用量减少到原工艺的四分之一,收率由78%提高到96%。设计并采用四氟对甲基苄醇先氯化得到四氟对甲基苄基氯,%,再与功夫酸反应制备七氟菊酯的新路线,%,,产品纯度大于96%。%%,获得了一条适合工业化合成七氟菊酯的工艺路线。关键词:四氯对苯二甲酸四氟对苯二甲酸二甲酯四氟对甲基苄醇,四氟对甲基苄基氯,功夫酸,,&thelefluthrinandthe4-methyl-2,3,5,6-tetrafluoro-tmnzylalcohol,a/iimportantintermediatefortefluthrin,-Methyl·2,3,5,·benzylalcoholwassynthesizedbyacylation,fluorination,esterifleation,reduction,bromizationandreductionfromtetracloro-(Z)-(IRS,3RS卜3·(2-chloro一3,3,3一trifluom—l·pmpenyl)·22一dimethylcycolpropaneearboxylateacidbyreactingwith4-chlormethyi-2?356-tetrafluorotoluolwhichwaspreparedfrom4-methyl-2,3,5,6-tctrafluom··bromicacidtoobtain(4-(bromomethyl)-2。356-tetrafluorophenyl),%%.4-Methyl-2,3,5,6-tetrafluoro-,theamountofmagnesiumdecreasedtoonefourthofthatinformermethodandtheyieldincreasedfrom78%to96%.-Methyl-2?356一Tetrafluombenzylchloridewaspreparedfrom4-methyl-2,3,5,6-tetrafluoro-%.Thentefluthrinwasachievedbythesubstitutedreactionof4-methyl一2?356-tetrafluoro—benzylchlorideand(z)·(19S,3RS)-3一(2·chloro·3,3