N-甲基-2-(3,4-二羟基苯基)[60]富勒烯吡咯烷衍生物的合成

Synthesis of N-Methyl-2-(3,4-dihydroxyphenyl)[60] Fullerene Pyrrolidine

在N2气保护下,由1,3-偶极环加成反应合成了含2个羟基的C60吡咯烷衍生物:N-甲基-2-(3,4-二羟基苯基)[60]富勒烯吡咯烷。用UV-Vis、FT-IR、1H NMR、MS等测试技术表征了产物的结构,通过单因素方法,探讨了反应条件对产物产率的影响。最佳反应条件为:n(C60)∶n(N-甲基甘氨酸)∶n(3,4-二羟基苯甲醛)=1∶2∶5,温度为95℃,反应时间为28 h,产率可达66%(以消耗的C60计)。

N-methyl-2-（3,4-dihydroxyphenyl） fullerene pyrrolidine was synthesized by the 1,3-dipolar cycloaddition reaction of fullerene（C60） and azomethine ylide（prepared from N-methylglycine and 3,4-dihydroxybenzaldehyde）.The product was characterized by UV-Vis,FI-IR,^1H NMR and MS.The reaction conditions affecting the yield were investigated and the optimum reaction conditions which afforded 66%（based on consumed C60） of the product were： molar ratio of C60∶N-methylglycine∶3,4-dihydroxybenzaldehyde 1∶2∶5,reaction temperature 95 ℃,reaction time 28 h.