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首页> 外文期刊>Zeitschrift fur Naturforschung, B. A Journal of Chemical Sciences >A new synthesis of tetrakis(C-methyl)octakis(hydroxyethyl)calix[4]-resorcinarene via an ethoxy-tethered trimethylsiloxy precursor
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A new synthesis of tetrakis(C-methyl)octakis(hydroxyethyl)calix[4]-resorcinarene via an ethoxy-tethered trimethylsiloxy precursor

机译:通过乙氧基拴三甲基硅氧烷前体进行新的四(C-甲基)octakis(羟乙基)℃(羟乙基)℃[4] -Resorcinarene的新合成

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摘要

The octakis(trimethylsiloxy)calix[4]resorcinarenes, 3 and 4, were synthesized by reaction of I. and its tetsabromo derivative 2 with hexamethyldisilazane, and were found to exhibit dynamic behaviour in solution. Temperature-dependent NMR investigations confirmed the presence of at least two conformational isomers of 3 in solution. The conformation of 3 in the solid state was determined by an X-ray crystal structure analysis; the calixarene displays a boat conformation. The introduction of the ethoxy group as a spacer into the molecule of 1 was effected via its reaction with ethyl bromoacetate and subsequent reduction with lithium aluminium hydride forming the ethoxy-tethered C-methylcalix[4]resorcinarene 6 in an impure state. Reaction of crude 6 with hexamethyldisilazane furnished the ethoxy-tethered octakis(trimethylsiloxy)calix[4]resorcinarene 7; its hydrolysis led to pure 6. [References: 27]
机译:通过I.及其Tetsabromo衍生物2与六甲基二硅氮烷的反应合成Octakis(三甲基硅氧烷)CALIX [4]反弹素,3和4,并发现在溶液中表现出动态行为。 温度依赖性NMR调查证实了在溶液中存在至少两个构象异构体。 通过X射线晶体结构分析确定固态中3的构象; Calixarene显示船只构象。 通过其与溴乙酸乙酯的反应和随后用氢氧铝酸锂的氢化锂的反应以纯度的状态进行乙氧基铝酸锂的乙氧基的引入作为间隔物。 粗r6与六甲基二硅氮烷的反应提供了乙氧基 - 系环八烷基(三甲基硅氧烷)CALIX [4]间苯二酚7; 它的水解导致纯6. [参考文献:27]

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