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當前位置:首頁公司新聞Syrris全自動超低溫合成儀*

Syrris全自動超低溫合成儀*

更新時間:2015-05-06點擊次數(shù):2583

超低溫反應是有機合成研究者經常會遇到的反應,比如丁基鋰拔氫和溴、Birch反應均要冷卻到-78°C下進行,如此低的反應溫度,經常讓研究者因如何搭建低溫反應裝置而頭疼。


目前普遍使用的低溫方法非常原始和粗糙,即通過一個杜瓦瓶作為保溫杯,用液氮或干冰作為冷卻介質,研究者通過溫度計來探測溫度,決定是否需要添加冷卻介質。該方法在研究反應可行性方面起到了一定的積極作用,但其缺陷嚴重,主要總結為以下幾個方面:

1、  溫度波動大,對反應不利,副產物增多;

2、  只能完成簡單的實驗操作,局限性大;

3、  反應重現(xiàn)性差;

4、  只能做小量的反應,對中式或放大指導意義不大;

5、  實驗員工作量大,需要不斷補給低溫介質,不適合耗時長的反應。

因此,該方法已經遠遠不能適應當今有機合成研究的要求了。隨著科技的的進步,超低溫循環(huán)油浴在一定程度上解決了低溫反應的難處,但也因其固有的局限性不能滿足實驗者的各種需求,主要表現(xiàn)在以下幾個方面:

1、  超低溫循環(huán)油浴并非反應釜,實驗者需要在油浴上手動搭建反應裝置,靈活性差,不能完成操作復雜的反應,無法實現(xiàn)自動化;

2、  如果實驗者需要做全自動合成完成復雜的反應,需要額外購買全自動合成儀配合使用,但價格非常昂貴,難以普及。


針對以上低溫反應的瓶頸,英國Syrris公司新推出Atlas超低溫合成儀,極大解決了研究者做低溫反應遇到的各種問題,通過電冷卻,可達-10℃到-80℃的溫度,無需任何冷卻介質(液氮、干冰、硅油),兼容實驗室zui常使用的圓底燒瓶,同時,可連接Atlas軟件和其它模塊,完成更加復雜的合成功能,如設定溫度加料,pH監(jiān)測和控制。目前,該技術**,*國內低溫合成儀器的空白。


詳細信息請登錄:

 http://syrris.com/batch-products/atlas-cryo-reactor


Atlas超低溫合成儀的應用:

1、  丁基鋰拔溴后的取代反應

 

有機合成中利用率zui高的低溫反應就是丁基鋰試劑參與的這種取代反應,正丁基鋰n-C4H9Li在-70°C的低溫下拔取噻吩環(huán)上的溴,大約耗時1h,然后與溴代物進行耦合。利用Atlas超低溫合成儀,的溫度控制使拔溴過程的副產物少,通過注射泵抽取正丁基鋰到反應瓶中,避免了正丁基鋰與空氣中的氧和水分接觸而自燃。


2、Birch還原反應

 

由于Na溶于液氨中會比發(fā)生較劇烈的放熱反應,因此把溫度控制在-78°C很重要,利用Atlas超低溫合成儀,可以的控制反應溫度。


Atlas超低溫合成儀還可運用在以下幾類低溫反應中:

1、  格氏反應

2、  傅-克反應

3、  邁克爾加成

4、  重氮化反應

5、  羥醛縮合反應


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