The six-, eight- and twelve-membered cyclo-siloxanes, cyclo-[R2SiOSi(Ot-Bu)(2)O](2) (R = Me (1), Ph (2)), cyclo-(t-BUO)(2)-Si(OSiR2)(2)O (R = Me (3), Ph (4)), cyclo-R2Si[OSi(Ot-Bu)(2)](2)O (R = Me (5), Ph (6)) and cyclo-[(t-BuO)(2)Si(OSiMe2)(2)O](2) (3a) were synthesized in high yields by the reaction of (t-BUO)2Si(OH)2 and [(t-BuO)(2)SiOH](2)O with R2SiCl2 and (R2SiCl)(2)O (R = Me, Ph). Compounds 1-6 were characterized by solution and solid-state Si-29 NMR spectroscopy, electrospray mass spectrometry and osmometric molecular weight determination. The molecular structure of 4 has been determined by single crystal X-ray diffraction and features a six-membered cyclo-siloxane ring that is essentially planar. The reduction of 1-6 with i-Bu2AlH (DIBAL-H) led to the formation of the metastable aluminosiloxane (t-BUO)(2)Si(OAli-Bu-2)(2) (7) along with Me2SiH2 and Ph2SiH2.
三甲基甲硅烷氧基三叔丁氧基硅烷 (I)、双(三甲基甲硅烷氧基)二叔丁氧基硅烷 (II) 和双(三甲基甲硅烷氧基)双(三叔丁氧基甲硅烷氧基)硅烷 (III) 是通过三甲基氯硅烷与三叔丁氧基硅烷反应制备的-丁氧基硅烷醇、二叔丁氧基硅烷二醇和双(三叔丁氧基甲硅烷氧基)硅烷二醇。双(三叔丁氧基甲硅烷氧基)二甲基硅烷(IV)也通过二甲基二氯硅烷与三叔丁氧基硅烷醇的反应获得。二甲基二氯硅烷与二叔丁氧基硅烷二醇或双(三叔丁氧基甲硅烷氧基)硅烷二醇的反应得到四甲基四叔丁氧基(V)或四甲基四(三叔丁氧基甲硅烷氧基)环辛硅氧烷(VI)。这些化合物通过元素分析、分子量测定以及 IR 和 NMR 光谱的研究进行鉴定。
Alkoxysilanes. VII. The Preparation of Alkylalkoxysiloxanes
作者:Ichiro Kijima、Keisuke Okuda、Yoshimoto Abe
DOI:10.1246/bcsj.44.1106
日期:1971.4
Trimethylsiloxytri-t-butoxysilane (I), bis(trimethylsiloxy)di-t-butoxysilane (II), and bis(trimethylsiloxy)bis(tri-t-butoxysiloxy)silane (III) were prepared by the reaction of trimethylchlorosilane with tri-t-butoxysilanol, di-t-butoxysilanediol, and bis(tri-t-butoxysiloxy)silanediol respectively. Bis(tri-t-butoxysiloxy)dimethylsilane (IV) was also obtained by the reaction of dimethyldichlorosilane
三甲基甲硅烷氧基三叔丁氧基硅烷 (I)、双(三甲基甲硅烷氧基)二叔丁氧基硅烷 (II) 和双(三甲基甲硅烷氧基)双(三叔丁氧基甲硅烷氧基)硅烷 (III) 是通过三甲基氯硅烷与三叔丁氧基硅烷反应制备的-丁氧基硅烷醇、二叔丁氧基硅烷二醇和双(三叔丁氧基甲硅烷氧基)硅烷二醇。双(三叔丁氧基甲硅烷氧基)二甲基硅烷(IV)也通过二甲基二氯硅烷与三叔丁氧基硅烷醇的反应获得。二甲基二氯硅烷与二叔丁氧基硅烷二醇或双(三叔丁氧基甲硅烷氧基)硅烷二醇的反应得到四甲基四叔丁氧基(V)或四甲基四(三叔丁氧基甲硅烷氧基)环辛硅氧烷(VI)。这些化合物通过元素分析、分子量测定以及 IR 和 NMR 光谱的研究进行鉴定。
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作者:Jens Beckmann、Dainis Dakternieks、Andrew Duthie、Edward R. T. Tiekink
The six-, eight- and twelve-membered cyclo-siloxanes, cyclo-[R2SiOSi(Ot-Bu)(2)O](2) (R = Me (1), Ph (2)), cyclo-(t-BUO)(2)-Si(OSiR2)(2)O (R = Me (3), Ph (4)), cyclo-R2Si[OSi(Ot-Bu)(2)](2)O (R = Me (5), Ph (6)) and cyclo-[(t-BuO)(2)Si(OSiMe2)(2)O](2) (3a) were synthesized in high yields by the reaction of (t-BUO)2Si(OH)2 and [(t-BuO)(2)SiOH](2)O with R2SiCl2 and (R2SiCl)(2)O (R = Me, Ph). Compounds 1-6 were characterized by solution and solid-state Si-29 NMR spectroscopy, electrospray mass spectrometry and osmometric molecular weight determination. The molecular structure of 4 has been determined by single crystal X-ray diffraction and features a six-membered cyclo-siloxane ring that is essentially planar. The reduction of 1-6 with i-Bu2AlH (DIBAL-H) led to the formation of the metastable aluminosiloxane (t-BUO)(2)Si(OAli-Bu-2)(2) (7) along with Me2SiH2 and Ph2SiH2.