Buckybowls on metal surfaces:: Symmetry mismatch and enantiomorphism of corannulene on cu(110)
Buckybowls on metal surfaces:: Symmetry mismatch and enantiomorphism of corannulene on cu(110)
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DOI：
10.1002/anie.200700610
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发表时间：
2007-01-01
影响因子：
16.6
通讯作者：
Siegel, Jay S.
中科院分区：
文献类型：
--
作者：
Parschau, Manfred;Fasel, Roman;Siegel, Jay S.
Rabiedau等人的方法的修改。[1]用于制备corannulene。用锌和碘化钾在DMF中代替盐酸和乙醇处理1，2，5，6-四溴corannulene，并将反应混合物在160 ℃下加热约24-36小时（TLC控制）。除去溶剂后，将残余物用CH 2Cl 2稀释并通过3cm厚的硅藻土层过滤。除去滤液中的溶剂，将浅黄色固体进行硅胶层析。用己烷/CH 2Cl 2（10/1）洗脱得到浅黄色固体状的corannulene（65-70%）。在~ 20 ℃下从乙醚中结晶，得到标题化合物，为浅黄色晶体。(b)LEED结果
A modification of the method of Rabiedau et al.[1] was used for the preparation of corannulene. 1, 2, 5, 6-Tetrabromocorannulene was treated with zinc and potassium iodide in DMF, instead of hydrochloric acid and ethanol, and the reaction mixture was heated at 160 ºC for~ 24-36 hours (TLC control). After removal of solvents, the residue was diluted with CH2Cl2 and filtered through a 3 cm thick layer of celite. The solvent of the filtrate was removed and the pale-yellow solid was subjected to chromatography on silica gel. Elution with hexane/CH2Cl2 (10/1) afforded corannulene (65-70%) as a light yellow solid. Crystallization from ether at~ 20 ºC gave the title compound as light yellow crystals.(b) LEED results