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1、1.Philosophy(安排)A.Numberofreactionsperday:>2(每天要進(jìn)行的反應(yīng):>2)B.Progress:daily(進(jìn)展:每日)C.Solution:weekly(解決方案:每周)D.Freetime(空閑時(shí)間)1.setupanotherreaction(開始另一種反應(yīng))2.Cleanglassware(清潔玻璃器皿)3.Completemiscellaneousmenialchores(完成各種瑣碎的小事)4.Read(閱讀)E.Cautionvs.speed(謹(jǐn)慎vs
2、.速度)1.Cutcornerswhenappropriate(在適當(dāng)?shù)臅r(shí)候加快進(jìn)度)2.Knowwhatcornershanvebeencut(知道哪些實(shí)驗(yàn)程序可以縮減)3.Slowdownwhennecessary(必要時(shí)減慢)Ⅱ.Planningtheexperiment(規(guī)劃實(shí)驗(yàn))A.Multiple/parallelreactions(多個(gè)/平行反應(yīng))1.Unrelatedreactions:overlap(juggle)whenpossible(無關(guān)的反應(yīng):可能重疊(歪曲))2.Related
3、reactions:runinparallel(相關(guān)的反應(yīng):平行的進(jìn)行)B.Scale(稱量)1.TCL:50-100μg(TCL:50-100μg)2.Smallpreparative:0.5-10mg(小規(guī)模的準(zhǔn)備:0.5-10毫克)3.Preparative:10-1.0mg(準(zhǔn)備:10-1.0毫克)4.Macroscale:>1.0g(大量稱量:>1.0克)C.Scale-up(規(guī)?;?.≦3-5fold≦3-5折疊2.Avoidlargescaleprep-evenliteratureprep
4、s-onfirstattempt避免在第一次嘗試時(shí)進(jìn)行大量的準(zhǔn)備Rule1:Neverchangethereactionconditionssubstantiallyonanimportantscale-up.大體上反應(yīng)是按比例的增加時(shí)永遠(yuǎn)不要改變反應(yīng)條件Assumethatachangeinconditionswillcausecompletefailureofthereactionandascertainwhetherthequantityofsubstrateisexpendable.假設(shè)條件的變化
5、將徹底導(dǎo)致的反應(yīng)失敗,并弄清楚底物的量是否是值得消耗。Rule2:Minimizescalewithinreason.在合理的范圍內(nèi)最大限度地減少的量的使用。Microscaleisfaster(videinfra)andconsumelessmaterial,微小的規(guī)模反應(yīng)快(參閱以下),并消耗更少的材料,Microscaleallowsyoutoworkatthefrontofthesynthesislonger.微小的規(guī)??梢宰屇诤铣擅媲肮ぷ鞲L時(shí)間。Rule3:You’renotmakingpr
6、ogressofyou’renotworkingatthefrontofthesynthesis.Bringingupstaringmaterialsisnotmakingprogress.你不在合成的過程中盯著工作的情況是不能取得進(jìn)展。Ⅲ.Staringthereaction(Ⅲ.注意認(rèn)真觀察反應(yīng))A.Vessel(容器)1.Round-bottompipettesw/stirflea:50μg-≧2.0mg(圓底移液器W/攪拌器:50μg≧2.0mg)2.Kimblevialsw/stirflea:u
7、pto≧1g(金布爾小瓶W/攪拌器:≧1克)a.(KimbleScienceProducts:1-609-794-5561)(金布爾科學(xué)產(chǎn)品:1-609-794-5561)b.2ml,part#150852B.c.5ml,part#150855d.10ml,part#15085103.Round-bottomflasks:onlywhennecessary(圓底燒瓶:只有當(dāng)需要的時(shí)候)B.Covers(蓋子)1.RBpipettes/Kimblevials:septaorNMRcaps(RB移液器/金布爾
8、小瓶:隔片或核磁共振蓋)2.Flasks:septaorgasadapter.(燒瓶:隔片或氣體適配器。)3.Sealedtubereaction:(tube管的反應(yīng))a.Kimblevialsw/NMRcaps(金布爾小瓶W/核磁共振蓋)b.RBflaskw/gasadaptor(經(jīng)常瓶W/天氣適配器)c.SealedNMRtubeor1/4tubing(密封的NMR管或1/4管)d.“bomb”w/Teflonjoint(