Synthesis, Multinuclear NMR Spectra, and X-ray Structures of tBu2PNP(I)tBu2 and EPR2NP(I)R2 (E = Se, Te; R = iPr, ts

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• 作者：Jamie S. Ritch ; Stuart D. Robertson ; Maarit Risto ; Tristram Chivers
• 刊名：Inorganic Chemistry
• 出版年：2010
• 出版时间：May 17, 2010
• 年：2010
• 卷：49
• 期：10
• 页码：4681-4686
• 全文大小：769K
• 年卷期：v.49,no.10(May 17, 2010)
• ISSN：1520-510X

文摘

Two synthetic routes to bifunctional P(V)/P(V) compounds of the type EPR<sub>2sub>NP(I)R<sub>2sub> have been developed. The reaction of Li[EP<sup>isup>Pr<sub>2sub>NP<sup>isup>Pr<sub>2sub>] with one molar equivalent of I<sub>2sub> produces EP<sup>isup>Pr<sub>2sub>NP(I)<sup>isup>Pr<sub>2sub> (3a-I, E = Se; 3b-I, E = Te). Alternatively, the oxidation of Na[N(P<sup>tsup>Bu<sub>2sub>)<sub>2sub>] with I<sub>2sub> in tetrahydrofuran (THF) generates the P(III)/P(V) compound <sup>tsup>Bu<sub>2sub>PNP(I)<sup>tsup>Bu<sub>2sub> (6′-I) which, on treatment with elemental selenium or tellurium in THF, yields EP<sup>tsup>Bu<sub>2sub>NP(I)<sup>tsup>Bu<sub>2sub> (3a′-I, E = Se; 3b′-I, E = Te). The acyclic compounds 3a-I, 3a′-I, 3b-I, 3b′-I, and 6′-I have been characterized in solution by multinuclear (<sup>1sup>H, <sup>31sup>P, <sup>77sup>Se, and <sup>125sup>Te) NMR spectroscopy and in the solid state by X-ray structural determinations.