Dalton Trans. 2013 Oct 7;42(37):13747-53. doi: 10.1039/c3dt51373d. Epub 2013 Aug 1.
Metal halides, solvent effects, phase transfer catalysts, alkylating agent and reaction times were found to have important roles to complete halogen exchange reactions in "one pot" synthesis, starting from octakis(3-chloropropyl)octasilsesquioxane to obtain more reactive halide compounds: octakis(3-bromopropyl)octasilsesquioxane and octakis(3-iodopropyl)octasilsesquioxane. To confirm the complete halogen exchange, the desired products were characterized by (1)H, (13)C and (29)Si NMR spectroscopy, ESI-MS, elemental analysis and single-crystal X-ray diffraction analysis.
金属卤化物、溶剂效应、相转移催化剂、烷基化试剂和反应时间在“一锅法”合成中对完成卤素交换反应起着重要作用，从八（3-氯丙基）八硅倍半氧烷出发，得到更具反应性的卤化物化合物：八（3-溴丙基）八硅倍半氧烷和八（3-碘丙基）八硅倍半氧烷。为了确认完全的卤素交换，通过（1）H、（13）C 和（29）Si NMR 光谱、ESI-MS、元素分析和单晶 X 射线衍射分析对所需产物进行了表征。
