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1、越般彭⑧天洋大謦中國(guó)近代第所大學(xué)碩士學(xué)位論文L'J-爿■●■■0●爿，}■■疆■■¨a____學(xué)科專(zhuān)業(yè)：亙刖t學(xué)作者姓名：盂祥啟指導(dǎo)教師：張里塹豇教授壬津士堂研窯畢陴2006年1月摘要本論文是關(guān)于菊酯類(lèi)農(nóng)藥七氟菊酯的合成和工藝優(yōu)化的研究，重點(diǎn)優(yōu)化了重要中間體四氟對(duì)甲基芐醇的合成工藝，并對(duì)目標(biāo)產(chǎn)物七氟菊酯的合成路線進(jìn)行了改進(jìn)。以四氯對(duì)苯二甲酸為原料，經(jīng)酰氯化、氟化、酯化、還原、溴化、還原六步反應(yīng)合成了四氟對(duì)甲基芐醇。四氟對(duì)甲基芐醇再經(jīng)氯化、與(z)．ORS，3RS)．3．(2-氯·3，3，3-三氟丙-l一丙烯基)一2，2．二甲基
2、環(huán)丙甲酸(功夫酸)酯化合成了七氟菊酯。重點(diǎn)對(duì)工藝路線中溴化、還原反應(yīng)進(jìn)行了優(yōu)化。以甲苯為溶劑，四氟對(duì)苯二芐醇與氫溴酸反應(yīng)制得四氟對(duì)溴甲基芐醇，將氫溴酸的用量從四氟對(duì)苯二芐醇的摩爾量10倍降低至5倍，并且使產(chǎn)品收率從88．13％提高到90．07％。四氟對(duì)溴甲基芐醇被鎂粉和甲醇還原生成四氟對(duì)甲基芐醇，通過(guò)采用替代溶劑，將鎂粉的用量減少到原工藝的四分之一，收率由78％提高到96％。設(shè)計(jì)并采用四氟對(duì)甲基芐醇先氯化得到四氟對(duì)甲基芐基氯，收率為95．28％，再與功夫酸反應(yīng)制備七氟菊酯的新路線，收率為91．86％，避免了原工藝中價(jià)格昂貴的D
3、CC，產(chǎn)品純度大于96％。優(yōu)化后總收率從52．94％提高到60．10％，獲得了一條適合工業(yè)化合成七氟菊酯的工藝路線。關(guān)鍵詞：四氯對(duì)苯二甲酸四氟對(duì)苯二甲酸二甲酯四氟對(duì)甲基芐醇，四氟對(duì)甲基芐基氯，功夫酸，七氟菊酯ABSTRACT11碡synthesisoftefluthrin．whichisakindofpyrethroidpesticide，wasstudiedinthispaper．Thesyntheticprocess&thelefluthrinandthe4-methyl-2，3，5，6-tetrafluoro-tmnzy
4、lalcohol，a／iimportantintermediatefortefluthrin，wercimproved．4-Methyl·2，3，5，6．tetrafluoro·benzylalcoholwassynthesizedbyacylation，fluorination，esterifleation，reduction，bromizationandreductionfromtetracloro-tercphthalieacid．Tefluthrinwasobtainedfrom(Z)-(IRS，3RS卜3·(2-ch
5、loro一3，3，3一trifluom—l·pmpenyl)·22一dimethylcycolpropaneearboxylateacidbyreactingwith4-chlormethyi-2?356-tetrafluorotoluolwhichwaspreparedfrom4-methyl-2，3，5，6-tctrafluom·benzylalcoh01．ThereactionsofbromizationandreductioninthesyntheticprocessweTestudied．Tetrafluoroter
6、ephthalylalcoholwasbromatcdinthehydro·bromicacidtoobtain(4-(bromomethyl)-2。356-tetrafluorophenyl)methan01．Withtoluene鼢solvent,theamountofhydrobromicaciddecreasedfromtentimesofthetooloftetrafluomterephthalylalcoholtofivetimesandtheyieldincreasedfrom88．13％to90．07％．4-M
7、ethyl-2，3，5，6-tetrafluoro-benzylalcoholwasobtainedbyreducingthebromidewithmagnesiumandmethan01．Byreplacingmathanolwithdichlommethaneassolvent,theamountofmagnesiumdecreasedtoonefourthofthatinformermethodandtheyieldincreasedfrom78％to96％．Anewrouteoftefluthrinwasdesigne
8、d．4-Methyl-2?356一Tetrafluombenzylchloridewaspreparedfrom4-methyl-2，3，5，6-tetrafluoro-benzylalcoholandtheyieldwas91．86％．Thentefluthrinwasac
