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1、華中師范大學(xué)碩士學(xué)位論文殺菌劑肟菌酯和吡唑醚菌酯的合成工藝研究姓名：徐平平申請學(xué)位級別：碩士專業(yè)：農(nóng)藥學(xué)指導(dǎo)教師：楊光富201205⑨碩士學(xué)位論文MASTER’STHESIS中文摘要本文系統(tǒng)研究了甲氧基丙烯酸酯類殺菌劑肟菌酯和吡唑醚菌酯的合成工藝。甲氧基丙烯酸酯類殺菌劑具有高效、低毒、對環(huán)境友好等優(yōu)點，研究肟菌酯和吡唑醚菌酯的合成工藝對改善我國的落后的農(nóng)藥結(jié)構(gòu)，降低傳統(tǒng)殺菌劑對環(huán)境的污染有著非常重要意義。肟菌酯的合成工藝路線是以鄰甲基苯甲酸為起始原料：鄰甲基苯甲酸跟三甲基氰硅烷反應(yīng)得到鄰甲基苯甲酰氰，再在酸性條件下水解得到酰胺，用甲醇酯化后與甲氧基胺鹽酸鹽
2、肟化，用NBS溴化，最后與間三氟甲基苯乙酮肟縮合得到肟菌酯。通過優(yōu)化各步的反應(yīng)條件和提純方法，使合成工藝更接近于工業(yè)化，并降低了生產(chǎn)成本，提高了反應(yīng)收率。本文對吡唑醚菌酯的合成工藝進(jìn)行了研究，確定了最優(yōu)合成路線是以對氯苯胺和鄰硝基甲苯為原料。首先利用對氯苯胺合成對氯苯肼鹽酸鹽，再經(jīng)過環(huán)化和氧化得到中間體1．(4．氯苯基)．3．羥基吡唑，再與鄰硝基芐溴縮合后經(jīng)過還原得到N．羥基-N．2．[N．(4．氯苯基)．3．吡唑氧基甲基】．苯胺，再經(jīng)過?；图谆玫竭吝蛎丫?。其中本文報道的還原是利用鋅粉／醋酸銨體系進(jìn)行還原，跟文獻(xiàn)報道的鋅粉／氯化銨體系還原和高壓催化
3、氫化相比，減少了污染，提高了生產(chǎn)安全性并大大降低了成本。關(guān)鍵詞：肟菌酯：吡唑醚菌酯：合成工藝⑨碩士學(xué)位論文MASTER’STHESISAbstractnlisdissertationistostudythesynthesisprocessoftrifloxystrobinandpyraclostrobin．Tifloxystrobinandpyraclostrobinarenewtypesofstrobilurinfungicide，whichhavehigllactivity,lowtoxicityandenvironmentallyfriendly．I
4、tisverysignificanttodevelopthesynthesisprocessoftrifloxystrobinandpyraclostrobininordertoimprovethestructureoffuagisidein0111"countyanddecreasetheeffecttotheenviroment．Tifloxystrobinisobtainedstartingfrom2-methyl-benzoicacid，whichreact、)l，itllcyanotrimethysilane，andthearoylcyanide
5、isobtained．Thearoylcyanideviahydrolysisunderacidicconditions，esterification、Ⅳitllmethanol，reaction晰mmethoxyamine，bromizatedbyN-bromosuccinimide，andthencondensation．Throughimprovethe．reactionconditions，wegetthebestsynthesisprocessoftifloxystrobin,andreducedtogeneratecostandimprovet
6、hereactionyield．Inthepaper,thesynthesisprocessesofpyraclostrobinhasbeenresearched．Theoptimumsyntheticrouteismadefrom4一chloroanilineand2-methylnilrobenzene．Firstsynthesis4-chlorophenylhydrazinehydrochloridewith4-chloroaniline，aftercyclizationandoxidation,wegetthe1一(4一chlorophenyl)·
7、1H—pyrazol一3一01．Andthenviabromination，condensation,reduction,acylationandmethylation,pymclostrobinhasbeensynthesized．Wereductnitryltohydroxylamine謝mzinc／anamoniumacetate，Reductionwithzinc／ammoniumchloridesystemandhigh-pressurecatalytichydrogenationreportedintheliterature，adecrease
8、ofpollution,improvetheproductions
