第三期-顾振华

1、谈谈实验室安全和实验的个人体会,导师：麻生明研究员汇报人：顾振华,有机所枫林论坛,往者可谏来者可追,2,主要内容,实验室安全个人的实验科学的信誉问题GivingProperCredit,3,溶剂(1)对神经系统破坏：抑制神经系统的传导冲动功能，产生麻醉，神经系统障碍或引起神经炎等。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、松节油、煤油、丙酮、三氯甲烷、异丙苯等。(2)对肝脏机能损伤：损伤肝脏机能，引起恶心、呕吐、发烧、黄疸炎及中毒性肝炎；一般氯化烃类均会引起肝脏中毒现象。四氯化碳、氯仿、三氯乙烯、四氯乙烷、苯及其衍生物等。(3)对肾脏机能破坏：肾脏为毒物排

2、泄器官，故最易中毒，且因血氧量减少，亦足以使肾脏受害，发生肾炎及肾病。烃类之卤化物、苯及其衍生物、二元醇及其单醚类、四氯化碳、乙醇等。(4)对造血系统破坏：破坏骨髓造成贫血现象。苯及其衍生物(硝基苯)如甲苯、氯化苯、二元醇等。(5)对粘膜及皮肤刺激：刺激粘膜，使鼻粘膜出血，喉头发炎，嗅觉丧失或因皮肤敏感产生红肿、发痒、红斑及坏疽病等。三氯甲烷、醚、苯、丙酮、甲醇、石油、氯酚、二氯乙烯、四氯化碳等。,4,控温仪毛细管温度计、温度计套管核磁管高温高压反应,5,操作规范整洁、有章程（洗瓶、药品的存放(苯胺)，称量、取用(双层手套法、注射器的正确使用)、了解不同试剂的性质(液氨)）过柱溶剂的转移,溶剂

3、球的固定,防护镜不要“意气用事”试管,蒸馏“空中接力”,6,多借鉴别人的经验LiAlH4：Workupbestconductedby“1,2,3-method”for1.0gLiAlH4used,added1mLH2O(slowly)then2mLof10%aqueousNaOH,then3mLofH2O无故乱翻书8:2规则,7,全合成：广度,方法学：深度,2.Corey-Bakshi-ShibatareductionCorey-Chaykovsky-epoxidation(Corey-ylide)Corey-FuchsreactionCorey-KimoxidationCorey-Winte

4、rolefinSynthesis,3.CouplingReactionJohnF.Hartwig,根深则叶茂,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)

5、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.Se

6、zen:Duringthepastweek,IhavetriedtocontactprofessorSamesabouttheretractionofpaperswithoutanysuccess.Ihavereservedcopiesofexperimentaldata,whichsupporttheoriginalclaimsofthesepublications,butwasnotgivenachancetopresentthesedata.IamalsopreparedtoperformthereactionsunderthesupervisionofprofessorSamesifI

7、amgivenachance.“ColumbiaUniversityhasforbiddenSamestospeaktothemediaaboutSezenortheuniversitysinvestigation.ThescientistsSezenidentifiedasbeingabletoreproduceherworkarebothmembersoftheSamesgroup.TheydeclinedtoverifyherassertionsorotherwisespeakwithC&EN.,37,FourmorepapersarebeingretractedbyColumbiaUn

8、iversityProfessorofChemistry,DaliborSames.Sezenhascriedfoulovertheretractions,maintainingthatshehasneverbeenproperlynotifiedorconsulted.Whatsmore,sheclaimsnotonlythatherworkcanbereproducedbutthatithasbeenreproducedbyothermembersoftheSamesgroup(C&EN,March23).HerassertionscannotbeverifiedbecausenooneintheSamesgrouphasbeenwillingtospeakwithC&EN.SezennowalsoclaimsthatSamesdidnotusethepropercatalystswhentryingtoreproduceherwork.,38,小结,安全实验,讲究效率,科学信誉,要善于保护好自己,39,定风波莫听穿林打叶声苏轼三月七日沙湖道中遇雨。