含能富勒烯吡咯烷衍生物的合成及工艺研究

Study on the Synthetic Technology of Nitrofulleropyrrolidine

利用Prato反应合成分离出了新型含硝基富勒烯吡咯烷衍生物1,并对其工艺条件进行了研究,探讨了反应物计量比、温度及时间对产物1产率的影响,得到了合成产物1的最佳工艺条件:C60,间硝基苯甲醛和N-甲基甘氨酸的物质的量比为1∶1∶2,温度为100℃,反应时间为16h,此时产物1产率达到94.8%(以消耗的C60计).同时用UV-Vis,FT-IR,1HNMR,13CNMR和MS等光谱手段确定了产物1的分子结构.

A new nitrofulleropyrrolidine derivative 1 was prepared by the Prato reaction, and the effects of ratios of raw materials, temperature and reaction time on the reaction were studied. The optimum synthetic technology conditions with 94.8% yield （based on consumed C60） are： 1 ： 1 ： 2 of molar ratio of C60, m-nitrobenzaldehyde and N-methylglycine, 100 ℃ of reaction temperature, 16 h of reaction time. The structure of product 1 was characterized by UV-Vis, PT-IR, ^1H NMR, ^13C NMR and MS spectra.