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机械化学和溶液法的互补合成:1,2-二苯基乙二胺和黄芩素的混合物研究
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摘要
固态机械化学合成是指通过人工研磨或在球磨机中进行的化学反应~1,近年来得到了广泛的关注,并成功应用于许多领域,如超分子复合材料、超分子聚合物、金属药物和金属有机框架。~2我们通过液体辅助研磨的方法研究和筛选了不同比例的黄芩素和1,2-乙二胺的混合物。结果表明,只有黄芩素和1,2-乙二胺在1:1研磨时,形成了共晶。相反,黄芩素与1,2-乙二胺在溶液法时,出乎意料的生成了脱水产物,然而,共晶很难通过溶液法获得。
Solid-state mechanochemical synthesis, where chemical reactions are carried out by manual grinding or ball milling, is becoming more intensely studied research field, partly because it can promote reactions between solids quickly and quantitatively, with either no added solvent or liquid-assisted grinding(LAG).~(1,2) It has been successfully applied in many research areas, such as supramolecular synthesis of hydrogen-or halogen-bonded materials, clusters and polymers, metallodrugs and porous metal-organic frameworks.~3 Herein, we have investigated and screened the mixture components of 1,2-diphenylethylenediamine(1,2-DPEN) and baicalein(BE) by LAG grinding in stoichiometric ratios 1:1, 1:2 and 2:1. It is found that 1:1 cocrystal of BE and 1,2-DPEN was formed by grinding. On the contrary, by solution crystallization of 1,2-DPEN and BE, it is unexpected to obtain the reaction product, whereas the cocrystal is hard to obtain by solution method.
引文
1.(a)S.L James,C.J.Adams,C.Bolm,D.Braga,P.Collier,T.Fri??i?,F.Grepioni,K.D.Harris,G.Hyett,W.Jones,A.Krebs,J.Mack,L.Maini,A.G.Orpen,I.P.Parkin,W.C.Shearouse,J.W.Steed,D.C.Waddell,Chemical Society reviews 2012,41(1),413.(b)T.Fri??i?,W.Jones,Faraday Discussions 2007,136,167.
    2 .(a)T.Fri??i?,Chem.Soc.Rev.2012,41,3493.(b)P.J.Beldon,L.F i,R.S.Stein,A.Thirumurugan,A.K.Cheetham,T.Fri??i?,Angew.Chem.,Int.Ed.2010,49,9640.(c)H.L.Liu,Y.F.Xie,Z.G.Pan,A.Famulari,F.Guo,Z.F.Zhou,J.Martí-Rujas,Cryst.Growth Des.2014,14,6528.

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