CHINESE JOURNAL OF ENERGETIC MATERIALS
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甲苯的氟两相硝化反应研究(Ⅱ)
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易文斌(1979-),男,博士研究生,主要研究含能材料及有机医药、农药中间体的合成。e-mail: yiwenbin5@163.com

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国防科工委“十五”预研项目(40406020103)


Nitration of Toluene with Fluorous Biphasic System (Ⅱ)
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    制备了全氟辛基磺酸稀土金属盐(RE(OPf)3,RE=La,Sm,Eu,Tb,Yb,Lu),并研究了该催化剂作用下甲苯的氟两相硝化反应。考察了催化剂用量和带有不同配体的稀土金属催化剂对反应的影响。研究表明,Yb(OPf)3和C10F18分别是最好的催化剂和氟溶剂,以Yb(OPf)3为催化剂在C10F18中甲苯硝化反应得率为56%,对位选择性为45%。含有催化剂的氟相通过简单的相分离,就可回收利用。

    Abstract:

    The catalyst of rare earth(Ⅲ) perfluorooctanesulfonates(RE(OPf)3, RE=La, Sm, Eu, Tb, Yb, Lu) were prepared for the nitration of toluene in fluorous biphasic system. Perfluorohexane (C6F14), perfluoro- methylcyclohexane (C7F14), perfluorotoluene (C7F8), perfluorooctane (C8F18), perfluorooctyl bromide (C8F17Br) or perfluorodecalin (C10F18, cis and trans-mixture) were used as fluorous solvent respectively for this reaction. Effects of rare earth metal salts with different ligands and amount of the catalyst on the reaction were studied. The results show that Yb(OPf)3 and C10F18 are the best catalyst and fluorous solvent respectively. The yield of nitration of toluene is 56% by using Yb(OPf)3 as a catalyst and C10F18 as a fluorous solvent, and para-selectivity is 45%; By simple separation of the fluorous phase containing only catalyst, nitration can be repeated many times.

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易文斌,蔡春.甲苯的氟两相硝化反应研究(Ⅱ)[J].含能材料,2006,14(1):29-31.
YI Wen-bin, CAI Chun. Nitration of Toluene with Fluorous Biphasic System (Ⅱ)[J]. Chinese Journal of Energetic Materials, 2006, 14(1):29-31.

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  • 收稿日期: 2005-05-16
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  • 在线发布日期: 2011-11-04
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