說起N.N-二甲基甲酰胺(DMF)大家一定很熟悉,因其良好的溶解性和較高的沸點,是有機合成中常用的有機溶劑之一,有萬能溶劑之稱。通常DMF在空氣中和加熱至沸點的溫度下都很穩定,但在反應體係中卻可能不那麽穩定了。
事實上,DMF在堿性和酸性條件下都可以分解產生二甲胺,這可以看成是一個酰胺的水解反應。純DMF是沒有氣味的,有時會在反應體係中聞到魚腥味,[
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![](https://blog.wenxuecity.com/upload/album/7e/82/c1/99c27fc01175n4i7UVx3.gif)
當酸水解然後用陰離子交換樹脂中和。最終產品通過燒結漏鬥過濾蒸除溶劑拿到。結果發現產品中有不溶於水的固體顆粒。固體顆粒應該來自於樹脂。所以過濾時用膜過濾應該比較好。
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Palladiumoncarbon(Pd/C)frequentlyigniteswhenitfirstcomesincontactwithmethanol(andtoalesserextent,anyflammableorganicsolvent)andassuchrepresentsasignificantsafetyrisk.TheseproceduresarerecommendedwheneverPd/Cisusedinconjunctionwithhydrogengas. Hydrogenationusingaballoon: 1)Evacuatethereactionvessel(thisshouldhaveatleasttwoopenings)andbackfillwithaninertgas(nitrogenorargo...[
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Hazards:Hydrogenationreactionsposeasignificantfirehazardduetotheuseofflammablereagentsandsolvents.Suchreagentsincludepalladiumoncarbon(Pd/C),whichishighlyflammableandcanignitesolventsandhydrogen.Itisespeciallydangerousafterhavingbeenusedforthehydrogenation.Thepresenceofhydrogengasincreasestheriskofexplosion.閱讀全文]
Donotpouranychemicalsintothesink.[
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ThebehaviourofaminsonTLCsometimeisweird.Evenonepurecompound,anaminecanshowmorethanonespotwhenaneutraleluentsystemisemployed.Inthissituation,abasiceluentsystembyaddingbasesuchammoniaortriethylaminewillredresstheproblem.[
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nonereaction,mCPBAhasbeenusedforconvertingonealkenetooneepoxide.Afterthereaction,theexcessmeta-Chloroperoxybenzoicacidshouldnotbepouredintotheorganicwastebarrel.[
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Formonitoronereaction,TLCshouldbethefirstconsideration.DonotrelayonNMRformonitoringonereaction.[
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Hastebringsnosuccess;hastemakeswaste;morehaste,lessspeed.[
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Don'tMakeAnyDecisionWhenYouAreAngry.
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