A Triphenylene-Based Triptycene with Large Free Volume Synthesized by Zirconium-Mediated Biphenylation
A Triphenylene-Based Triptycene with Large Free Volume Synthesized by Zirconium-Mediated Biphenylation
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DOI：
10.1021/jo801643u
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发表时间：
2009-01-02
影响因子：
3.6
通讯作者：
King, Benjamin T.
中科院分区：
文献类型：
--
作者：
Hilton, Cameron L.;Jamison, Christophcr R.;King, Benjamin T.
以（Li（THF）（4））（2）中心点Zr（bphe）（3）为中心，将桥端带有H（1-H）或Bu（1-Bu）的六溴三蝶烯进行联苯化反应，得到了带有苯并菲叶片的三蝶烯。叶片垂直于和平行于3重轴延伸，并产生大的分子内自由体积（IMFV）（1-H，AM 1，710埃（3）;参见。三蝶烯，AM 171埃（3））。不能获得1-H的晶体。三蝶烯1-Bu是结晶的，其中Bu基团填充桥头附近的空隙。X-射线衍射分析表明，晶体包装与交替联锁波纹和扭曲的六方层。
Biphenylation using (Li(THF)(4))(2)center dot Zr(biphe)(3) of hexabromotriptycenes bearing H (1-H) or Bu (1-Bu) at the bridgeheads gave triptycenes with triphenylene blades. The blades extend both perpendicular and parallel to the 3-fold axis and generate a large intramolecular free volume (IMFV) (1-H, AM1, 710 angstrom(3); cf. triptycene, AM1 71 angstrom(3)). Crystals of 1-H Could not be obtained. Triptycene 1-Bu, in which the Bu (groups fill the voids near the bridgehead, was crystalline. X-ray diffraction analysis revealed crystal packing with alternating interlocked corrugated and distorted hexagonal layers.