离子液体载催化剂在医药中间体环戊烷并吡啶合成的应用

The application ionic liquid anchored catalyst in synthesis of pharmaceutical intermediate 2, 3-cyclopentenopyridine

以氯代正丁烷、N-甲基咪唑和氯化铜为原料，制备了离子液体载催化剂BMImCuCl3，通过红外光谱和核磁共振波谱对其结构进行了表征，研究了其在催化环戊酮与丙炔胺环合成环戊烷并吡啶反应中的应用。结果表明，较为合适的催化体系为BMImBF4／BMImCuCl3，催化剂BMImCuCl3的用量为10％，反应物摩尔比为1：1．5，反应温度为60℃，反应时间为3h，收率达67．3％。该离子液体催化体系循环使用3次，催化活性没有明显降低。与传统合成方法相比，在离子液体中的合成方法具有反应时间短、选择性和收率高，离子液体载催化剂可以循环使用等优点。

Ionic liquid anchored catalyst BMImCuCl3 was prepared from chlorobutane, N-methyl imidazolium and CuCl2, the structure was characterized by IR and ^1H-NMR, and the application in the synthesis of 2, 3-cyclopenteno-pyridrine was studied. The optimum reaction conditions were established by single factor experiments as follows： the suitable solvent and catalyst system is BMImBF4/BMImCuCl3, the addition amount of catalyst is 10%, the mole ratio of cyclopentanone and propargylamine is 1 ： 1.5, the reaction temperature is 60℃, the reaction time is 3.0h, under which conditions 2, 3-cyclopentenopyridine was obtained in 67.3% yield. The ionic liquid system was easily to be recycled at least 3 times without any activity loss. Compared with literature method, the manifest advantages including short reaction times, high selectivity and yield, simple isolation process, ease of recycle of ionic liquid system had been observed in the novel method.