An Efficient Route for the Synthesis of a Tin(II) Substituted Carbodiimide from a Diazo Compound

The reaction of β-diketiminate substituted tin(II) chloride, LSnCl (1; L = HC{(CMe)(2,6-iPr2C6H3N)}2), with the lithium salt of trimethylsilyl diazomethane (LiC(N2)SiMe3) is described. In the course of the reaction, the exclusive formation of tin(II) substituted carbodiimide LSnNCNSiMe3 (2) is observed in good yield. This reaction occurs at room temperature without any side products. Furthermore, we reacted diiron nonacarbonyl, Fe2(CO)9, with compound 2 to confirm the carbodiimide skeleton (NCN) without rearrangement. The latter reaction leads to the tin(II) coordinate iron carbonyl complex LSnNCNSiMe3Fe(CO)4 (3). Compounds 2 and 3 were investigated by microanalysis and multinuclear NMR spectroscopy and were further characterized by X-ray structural analysis.

本文报道了β-二亚胺基取代的氯化锡(II)（β-diketiminate substituted tin(II) chloride，LSnCl，化合物1；其中配体L = HC{(CMe)(2,6-二异丙基苯基氨基)}2）与三甲基硅基重氮甲烷（trimethylsilyl diazomethane）的锂盐（LiC(N2)SiMe3）的反应。反应过程中，以良好收率专一生成锡(II)取代的碳二亚胺LSnNCNSiMe3（化合物2），该反应在室温下进行且无任何副产物生成。此外，为验证碳二亚胺骨架（N=C=N）未发生重排，我们将九羰基二铁（diiron nonacarbonyl，Fe2(CO)9）与化合物2进行反应，最终得到锡(II)配位的羰基铁配合物LSnNCNSiMe3Fe(CO)4（化合物3）。通过元素分析（microanalysis）、多核核磁共振波谱（multinuclear NMR spectroscopy）对化合物2和3进行了表征，并进一步通过X射线晶体结构分析（X-ray structural analysis）确认了其结构。