Institute of Chemical Research, Kyoto University, Uji 611-0011, Kyoto, Japan.
Philos Trans A Math Phys Eng Sci. 2013 Aug 5;371(1998):20110636. doi: 10.1098/rsta.2011.0636. Print 2013 Sep 13.
The first synthesis of endohedral fullerene containing molecular hydrogen, H₂@C₆₀, is briefly summarized. The synthesis was conducted according to what we call the 'molecular surgical method', that is, opening a hole on a C₆₀ surface, enlargement of the hole, insertion of a guest species and enclosure of the hole without loss of the encapsulated guest. The entire process involves three chemical reactions to open the hole and four reactions to gradually reduce the hole size and finally close the hole. The total yield of the product, H₂@C₆₀, based on consumed C₆₀ was 9%. The encapsulated molecule of hydrogen exhibited a 6 ppm upfield-shifted ¹H NMR signal when compared with free hydrogen, indicating the aromaticity at the inner centre of the C₆₀ cage.
简要总结了首例包含分子氢的笼状富勒烯，即 H₂@C₆₀ 的合成。该合成采用了我们所谓的“分子外科方法”，即在 C₆₀ 表面上开一个孔，扩大孔，插入客体物种并封闭孔，而不会丢失包裹的客体。整个过程涉及三个化学反应来打开孔，以及四个反应来逐渐缩小孔的大小，最后关闭孔。基于消耗的 C₆₀，产物 H₂@C₆₀ 的总产率为 9%。与自由氢相比，所包裹的氢分子的 ¹H NMR 信号向低场移动了 6 ppm，表明 C₆₀ 笼内中心的芳香性。
