新型磁性纳米石墨烯的合成及其在有机合成中的应用
发布时间：2018-11-03 10:00
【摘要】：近几十年,催化剂在化学反应中所发挥的作用已经越来越受到化学家的关注,但是,大部分催化剂由于受到诸多条件的限制并不能得到广泛的应用,比如,昂贵的价格、循环利用率低、收率不高、分离回收困难等多种因素。尤其在制药领域,发展一种易回收,循环利用率高的催化剂是十分必要的。石墨烯因其独特的单原子厚度的二维结构,高的导电性和电荷迁移率,大的比表面积,优异的机械性能,热性能和电性能等优点,同时石墨烯在强氧化剂的作用下碳碳双键被氧化成一些含氧活性基团,如:环氧、羰基、羟基、羧基等,因此其深受化学工作者的青睐。由于石墨烯制备的催化剂不易回收,于是我们将石墨烯做成磁性材料,合成了新型磁性纳米催化剂Fe3O4@GO@Mo。在室温条件下双氧水的乙醚溶液中,将其用于环氧化合物开环反应,得到β-羟基过氧化物,产率较高。催化剂通过外加磁铁即可回收,且催化剂循环使用6次后其催化活性没有降低。随后,我们将新型磁性纳米催化剂Fe_3O_4@GO@Mo用于螺环吲哚类衍生物的合成。这种催化剂对于合成各种取代基的螺环吲哚类衍生物具有不错的催化效果。该反应由靛红衍生物、丙二腈和4-(苯基氨基)呋喃-2(3H)-酮类衍生物三组分为原料,在低共熔溶剂(氯化胆碱:尿素=1:2)中,微波加热的条件下反应,得到具有不同取代基的螺环吲哚类衍生物的终产物,收率较高。此方法以低共溶溶剂作为反应条件绿色无污染,并且溶剂可回收利用。我们还合成了新型磁性纳米催化剂Fe_3O_4@GO@SO_3H,用于吡唑并[3,4-b]吡啶类衍生物的合成。以5-氨基-1-苯基-3-(吡啶-3-基)-1H-吡唑、芳香醛、3-氧代-3-(吡啶-3-基)丙腈为原料,在低共溶溶剂(氯化胆碱:甘油=1:3)中,催化剂Fe_3O_4@GO@SO_3H存在的条件下80℃得到终产物吡唑并[3,4-b]吡啶衍生物,收率较高。并且磁性纳米材料的诸多优点如:制备简单、便于与产物分离和可循环利用等,都使得磁性纳米材料广泛应用于有机合成中成为可能。
[Abstract]:In recent decades, the role of catalyst in chemical reaction has been paid more and more attention by chemists. However, most of the catalysts can not be widely used because of the limitations of many conditions, such as high price. The recycling efficiency is low, the yield is not high, the separation and recovery are difficult and so on. Especially in pharmaceutical field, it is necessary to develop a catalyst which is easy to recycle and has high recycling efficiency. Graphene is characterized by its unique two-dimensional structure with monoatomic thickness, high conductivity and charge mobility, large specific surface area, excellent mechanical properties, thermal properties and electrical properties, etc. At the same time, graphene is oxidized to some oxygen-containing active groups under the action of strong oxidant, such as epoxy, carbonyl, hydroxyl, carboxyl, etc. Because the catalyst prepared by graphene is not easy to be recovered, we made graphene into magnetic material and synthesized a new magnetic nanometer catalyst Fe3O4@GO@Mo.. In the ether solution of hydrogen peroxide at room temperature, 尾 -hydroxyl peroxide was synthesized by ring opening reaction of epoxy compound in high yield. The catalyst can be recovered by adding magnets, and the catalytic activity of the catalyst does not decrease after 6 cycles. Subsequently, a novel magnetic nanometer catalyst Fe_3O_4@GO@Mo was used to synthesize spirocyclic indole derivatives. This catalyst has a good catalytic effect on the synthesis of various substituted derivatives of spirocyclic indole derivatives. The reaction was prepared from indirubin derivatives, malonitrile and 4- (phenylamino) furan-2 (3H) -ketone derivatives under microwave heating in a low eutectic solvent (choline chloride: urea = 1:2). The final product of spirocyclic indole derivatives with different substituents was obtained in high yield. In this method, low co-soluble solvent is used as the reaction condition, and the solvent can be recycled. We have also synthesized a new magnetic nanometer catalyst Fe_3O_4@GO@SO_3H, for the synthesis of pyrazole [3o 4 b] pyridine derivatives. Using 5-amino-1-phenyl-3- (pyridine-3-yl) -1H-pyrazole, aromatic aldehydes, 3-oxo-3- (pyridine-3-yl) propionitrile as raw materials, in a low soluble solvent (choline chloride: glycerol = 1:3), In the presence of catalyst Fe_3O_4@GO@SO_3H, pyrazolium pyridine derivatives were obtained at 80 鈩，
本文编号：2307463
[Abstract]:In recent decades, the role of catalyst in chemical reaction has been paid more and more attention by chemists. However, most of the catalysts can not be widely used because of the limitations of many conditions, such as high price. The recycling efficiency is low, the yield is not high, the separation and recovery are difficult and so on. Especially in pharmaceutical field, it is necessary to develop a catalyst which is easy to recycle and has high recycling efficiency. Graphene is characterized by its unique two-dimensional structure with monoatomic thickness, high conductivity and charge mobility, large specific surface area, excellent mechanical properties, thermal properties and electrical properties, etc. At the same time, graphene is oxidized to some oxygen-containing active groups under the action of strong oxidant, such as epoxy, carbonyl, hydroxyl, carboxyl, etc. Because the catalyst prepared by graphene is not easy to be recovered, we made graphene into magnetic material and synthesized a new magnetic nanometer catalyst Fe3O4@GO@Mo.. In the ether solution of hydrogen peroxide at room temperature, 尾 -hydroxyl peroxide was synthesized by ring opening reaction of epoxy compound in high yield. The catalyst can be recovered by adding magnets, and the catalytic activity of the catalyst does not decrease after 6 cycles. Subsequently, a novel magnetic nanometer catalyst Fe_3O_4@GO@Mo was used to synthesize spirocyclic indole derivatives. This catalyst has a good catalytic effect on the synthesis of various substituted derivatives of spirocyclic indole derivatives. The reaction was prepared from indirubin derivatives, malonitrile and 4- (phenylamino) furan-2 (3H) -ketone derivatives under microwave heating in a low eutectic solvent (choline chloride: urea = 1:2). The final product of spirocyclic indole derivatives with different substituents was obtained in high yield. In this method, low co-soluble solvent is used as the reaction condition, and the solvent can be recycled. We have also synthesized a new magnetic nanometer catalyst Fe_3O_4@GO@SO_3H, for the synthesis of pyrazole [3o 4 b] pyridine derivatives. Using 5-amino-1-phenyl-3- (pyridine-3-yl) -1H-pyrazole, aromatic aldehydes, 3-oxo-3- (pyridine-3-yl) propionitrile as raw materials, in a low soluble solvent (choline chloride: glycerol = 1:3), In the presence of catalyst Fe_3O_4@GO@SO_3H, pyrazolium pyridine derivatives were obtained at 80 鈩，
本文编号：2307463
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