Allyl Calcium Compounds: Synthesis and Structure of Bis(η3-1-alkenyl)calcium
Allyl Calcium Compounds: Synthesis and Structure of Bis(η3-1-alkenyl)calcium
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烯丙基钙化合物：双(η3-1-烯基)钙的合成和结构
DOI：
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发表时间：
2011
期刊：
影响因子：
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通讯作者：
J. Okuda
中科院分区：
文献类型：
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作者：
Phillip Jochmann;Stefanie Maslek;T. Spaniol;J. Okuda
不同链长的烯丙基钙化合物[Ca(R)2(THF)x] (x = 0.15−0.25 (1-Ca, 3-Ca), 0.25−0.75 (2-Ca))通过CaI2与烯丙基钾试剂[K(R)]的盐复分解合成(R = 正丁烯基(1-K)、异丁烯基(2-K)、正己烯基) (3-K))，由相应的α-烯烃和Schlosser碱制备。新的钙衍生物以接近定量的产率获得。 1-Ca 和 2-Ca 可以结晶为三甘醇二甲醚加合物（三甘醇二甲醚：三（乙二醇）二甲醚），并通过单晶 X 射线衍射进行结构表征。所有钾前体 [K(R)] 也被分离并通过 1H 和 13C NMR 光谱进行表征。 THF 中的溶液性质与所有分离化合物的烯丙基部分的 η3-配位模式一致。对于钾试剂 1-K 和 3-K，观察到 >99:<1 和 85:15 的内/外平衡分布，而对于钙化合物 1-Ca 和 3-Ca，在 25 °C 时分别发现 60:40 和 42:58 的分布。这个区...
Allyl calcium compounds of different chain lengths [Ca(R)2(THF)x] (x = 0.15−0.25 (1-Ca, 3-Ca), 0.25−0.75 (2-Ca)) were synthesized by salt metathesis of CaI2 with allylpotassium reagents [K(R)] (R = n-butenyl (1-K), isobutenyl (2-K), n-hexenyl (3-K)), prepared from the corresponding α-olefin and Schlosser base. The new calcium derivatives were obtained in nearly quantitative yields. 1-Ca and 2-Ca could be crystallized as triglyme adducts (triglyme: tris(ethylene glycol)dimethyl ether) and structurally characterized by single-crystal X-ray diffraction. All potassium precursors [K(R)] were also isolated and characterized by 1H and 13C NMR spectroscopy. The solution properties in THF are in agreement with an η3-coordination mode of the allyl moiety for all isolated compounds. For the potassium reagents 1-K and 3-K, endo/exo equilibrium distributions of >99:<1 and 85:15 were observed, whereas for the calcium compounds 1-Ca and 3-Ca, distributions of 60:40 and 42:58 were found at 25 °C, respectively. This distr...
影响因子：
15
作者：
Jain, Pankaj;Antilla, Jon C.
通讯作者：
Antilla, Jon C.
影响因子：
15
作者：
Han, Soo Bong;Gao, Xin;Krische, Michael J.
通讯作者：
Krische, Michael J.