（精選）第三期-顧振華.ppt

談?wù)剬?shí)驗(yàn)室安全和實(shí)驗(yàn)的個人體會,導(dǎo)師：麻生明研究員匯報(bào)人：顧振華,有機(jī)所楓林論壇,往者可諫來者可追,1,2,主要內(nèi)容,實(shí)驗(yàn)室安全個人的實(shí)驗(yàn)科學(xué)的信譽(yù)問題GivingProperCredit,3,溶劑(1)對神經(jīng)系統(tǒng)破壞：抑制神經(jīng)系統(tǒng)的傳導(dǎo)沖動功能，產(chǎn)生麻醉，神經(jīng)系統(tǒng)障礙或引起神經(jīng)炎等。酒精、苯、氯化乙醇、二氯乙烷、汽油、甲酸戊酯、醋酸戊酯、二甲苯、三氯乙烯、丁醇、松節(jié)油、煤油、丙酮、三氯甲烷、異丙苯等。(2)對肝臟機(jī)能損傷：損傷肝臟機(jī)能，引起惡心、嘔吐、發(fā)燒、黃疸炎及中毒性肝炎；一般氯化烴類均會引起肝臟中毒現(xiàn)象。四氯化碳、氯仿、三氯乙烯、四氯乙烷、苯及其衍生物等。(3)對腎臟機(jī)能破壞：腎臟為毒物排泄器官，故最易中毒，且因血氧量減少，亦足以使腎臟受害，發(fā)生腎炎及腎病。烴類之鹵化物、苯及其衍生物、二元醇及其單醚類、四氯化碳、乙醇等。(4)對造血系統(tǒng)破壞：破壞骨髓造成貧血現(xiàn)象。苯及其衍生物(硝基苯)如甲苯、氯化苯、二元醇等。(5)對粘膜及皮膚刺激：刺激粘膜，使鼻粘膜出血，喉頭發(fā)炎，嗅覺喪失或因皮膚敏感產(chǎn)生紅腫、發(fā)癢、紅斑及壞疽病等。三氯甲烷、醚、苯、丙酮、甲醇、石油、氯酚、二氯乙烯、四氯化碳等。,4,控溫儀毛細(xì)管溫度計(jì)、溫度計(jì)套管核磁管高溫高壓反應(yīng),5,操作規(guī)范整潔、有章程（洗瓶、藥品的存放(苯胺)，稱量、取用(雙層手套法、注射器的正確使用)、了解不同試劑的性質(zhì)(液氨)）過柱溶劑的轉(zhuǎn)移,溶劑球的固定,防護(hù)鏡不要“意氣用事”試管,蒸餾“空中接力”,6,多借鑒別人的經(jīng)驗(yàn)LiAlH4：Workupbestconductedby“1,2,3-method”for1.0gLiAlH4used,added1mLH2O(slowly)then2mLof10%aqueousNaOH,then3mLofH2O無故亂翻書8:2規(guī)則,7,全合成：廣度,方法學(xué)：深度,2.Corey-Bakshi-ShibatareductionCorey-Chaykovsky-epoxidation(Corey-ylide)Corey-FuchsreactionCorey-KimoxidationCorey-WinterolefinSynthesis,3.CouplingReactionJohnF.Hartwig,根深則葉茂,1.PhilBaranChemical(b)The1HNMRspectrumafter4hours;(c)The1HNMRspectrumafter6hours;(d)The1HNMRspectrumafter27hours,17,18,19,20,21,22,23,24,25,26,ORTEPrepresentationoftrans-96sc,27,28,29,Conditions:(a)C2H5Br,Mg,THF,thenacetylene;(b)CD3COCD3,34%;(c)NaH,Et2O,thenClCO2Me,71%;(d)n-BuLi,Et2O,-78oC;thenH2O,-78oC,38%;(d)2-allyl-4-phenylbuta-2,3-dienoicacid,Pd(OAc)2/TFP,K2CO3,DMSO,54%,95%D.,30,31,Theplausiblepathway,32,33,GivingProperCredit,Chemicalthustheseretractionscameasasurprisetome.Istronglyprotestthattheretractionsweremadewithoutmyknowledge.Sezen:Duringthepastweek,IhavetriedtocontactprofessorSamesabouttheretractionofpaperswithoutanysuccess.Ihavereservedcopiesofexperimentaldata,whichsupporttheoriginalclaimsofthesepublications,butwasnotgivenachancetopresentthesedata.IamalsopreparedtoperformthereactionsunderthesupervisionofprofessorSamesifIamgivenachance.“ColumbiaUniversityhasforbiddenSamestospeaktothemediaaboutSezenortheuniversitysinvestigation.ThescientistsSezenidentifiedasbeingabletoreproduceherworkarebothmembersoftheSamesgroup.TheydeclinedtoverifyherassertionsorotherwisespeakwithC&EN.,37,FourmorepapersarebeingretractedbyColumbiaUniversityProfessorofChemistry,DaliborSames.Sezenhascriedfoulovertheretractions,maintainingthatshehasneverbeenproperlynotifiedorconsulted.Whatsmore,sheclaimsnotonlythatherworkcanbereproducedbutthatithasbeenreproducedbyothermembersoftheSamesgroup(C&EN,March23).HerassertionscannotbeverifiedbecausenooneintheSamesgrouphasbeenwillingtospeakwithC&EN.SezennowalsoclaimsthatSamesdidnotusethepropercatalystswhentryingtoreproduceherwork.,38,小結(jié),安全實(shí)驗(yàn),講究效率,科學(xué)信譽(yù),要善于保護(hù)好自己,39,定風(fēng)波莫聽穿林打葉聲蘇軾三月七日沙湖道中遇雨。