烯丙基碳硅烷枝状分子的官能化

通过硅氢化加成及还原反应,将四烯丙基硅烷（G₀）官能化,制备端基为4个Si—H键的碳硅烷枝状分子。考察不同的催化剂、溶剂、投料方式及温度对官能化反应的影响,以及不同的流动相、床层体积及流速对硅胶柱层析分离效果的影响,并通过高效液相色谱（HPLC）、红外光谱（IR）和核磁共振氯谱（¹H-NMR）对分离产物进行表征。结果表明:采用H₂PlCl₆-C₃H₇OH为催化剂,四氢呋喃为溶剂,溶液式投料,滴加温度和后续反应温度已控制在0和35℃的条件下,制备端基为4个Si—H键的碳硅烷枝状分子,采用石油醚为洗脱剂,在床层为φ2.5 cm×35 cm,流速为2.0mL/min硅胶柱中对其进行分离纯化,总收率达到70.5%:经鉴定,产物结构完整,与理论结构相符合。

Functionalization of allylsilane carbosilane dendrimer

The carbosilane dendrimer with four Si—H bonds as terminal groups was prepared by the lunctionalization （hydrosilylation and reduction）of tetra-allysilane carbosilane dendrimer（G₀）.The effects of catalyst,system solvent,feeding mode and temperature on the lunctionalization,and the effects of mobile phase,bed volume and flow rate on the chromatography separation of silica gel column were investigated. The product was characterized by high performiance liquid chromatography（HPLC）,infrared spectroscopy （IR）and ¹H nuclear magnetic resonance（¹H-NMR）.Results showed that,when the optimized reaction conditions were H₂PtCl₆-i-C₃H₇OH（catalyst）,tetrahydrofuran（THF）as solvent,solution（feeding mode）and 0,35℃（drop-addition temperature/reaction temperature）in the functionalization,and with petroleum ether（mobile phase）,φ2.5 cm×35 cm（bed volume）and 2.0 mL/min（flow rate）in the silica gel column chromatography separation,the yield of all the routes reached 70.5%.The structure of the product was proved to be corresponding with the theoretical structure by the characterization.