二异丁基氢化铝Ⅰ(DIBAL-H Ⅰ)还原碘代苯甲醛的研究

Study on reduction of iodobenzaldehyde by diisobutyl aluminum hydride Ⅰ

利用二异丁基氢化铝Ⅰ(DIBAL-H Ⅰ)在反应进行时可以不破坏苯环上其他官能团的特性,由碘代苯甲醛与无水二氯甲烷外加溶解在甲苯中的二异丁基氢化铝溶液中的碘代苯甲醇(首先经过搅拌,然后向混合物中加入饱和的酒石酸钠水溶液,接下来通过萃取、洗涤、干燥等过程合成),然后对产物进行了核磁共振氢谱图、核磁共振碳谱图以及高分辨质谱(HR-MS)的分析。并与常用还原剂硼氢化钠做对比,在制备目标产物碘代苯甲醇时进行了平行实验,分别对反应温度,反应时间,反应溶剂进行筛选,结果证明,0℃为反应的最优温度。二氯甲烷为最优溶剂,2h为最佳反应时间的最优反应条件。

Diisobutyl aluminum hydride Ⅰ(DIBAL-H Ⅰ)can be used without damaging the characteristics of other functional groups on the benzene ring during the reaction. The aluminum hydride solution is first stirred, then a saturated sodium tartrate aqueous solution is added to the mixture, and then iodobenzyl alcohol is synthesized through extraction, washing, and drying processes, and then the product is subjected to nuclear magnetic resonance hydrogen spectrum and nuclear magnetic resonance carbon spectrum And high-resolution mass spectrometry(HR-MS)analysis, i And compared with the commonly used reducing agent sodium borohydride, we conducted parallel experiments when preparing the target product iodobenzyl alcohol, and screened the reaction temperature, reaction time,and reaction solvent. The results proved that 0℃ is the optimal temperature for the reaction. Dichloromethane is the optimal solvent, and 2 h is the optimal reaction condition for the optimal reaction time.