N-叔丁基-α-苯基硝酮的合成及表征

Synthesis and characterization of N-tert-Butyl-Alpha-phenylnitrone

目的研究优化N-叔丁基-α-苯基硝酮的合成方法。方法采用羰基化合物与胺脱水的方法,以苯甲醛,叔丁胺、氯过氧苯甲酸等为原料合成目标产物N-叔丁基-α-苯基硝酮(TM),通过熔点测定、核磁及质谱分析表征其化学结构,研究了不同溶剂、不同原料、不同反应摩尔比对转化率和纯度的影响。结果获得最优化的合成路线和处理方法,产物结构鉴定与N-叔丁基-α-苯基硝酮(TM)一致,纯度大于98%。结论采用此种合成方法成本低、纯度高,经济可行。

Objective To investigate optimal method of N-tert-butyl-alpha-phenylnitrone synthesis. Methods Benzaldehyde, tert-butylamine and chloroperbenzoic acid were used as materials to synthesize the target product N-tert-butyl-alpha-phenylnitrone（TM） through dehydration of carbonyl compounds and amine. Its chemical structure was characterized by melting point determination, nuclear magnetic resonance and mass spectrometry, to examine the effects of different solvents, materials and mole ratios on conversion rate and purity in the reaction. Results Optimized synthetic route and processing method were obtained from the present study. The structure of the product was identical to N-tert-butyl-alpha-phenylnitrone（TM）, and its purity was more than 98%. Conclusion This synthetic method has the advantages of low cost and high purity, and thus is economical and feasible.