新型磁性納米石墨烯的合成及其在有機合成中的應用
發(fā)布時間：2018-11-03 10:00
【摘要】：近幾十年,催化劑在化學反應中所發(fā)揮的作用已經(jīng)越來越受到化學家的關注,但是,大部分催化劑由于受到諸多條件的限制并不能得到廣泛的應用,比如,昂貴的價格、循環(huán)利用率低、收率不高、分離回收困難等多種因素。尤其在制藥領域,發(fā)展一種易回收,循環(huán)利用率高的催化劑是十分必要的。石墨烯因其獨特的單原子厚度的二維結構,高的導電性和電荷遷移率,大的比表面積,優(yōu)異的機械性能,熱性能和電性能等優(yōu)點,同時石墨烯在強氧化劑的作用下碳碳雙鍵被氧化成一些含氧活性基團,如:環(huán)氧、羰基、羥基、羧基等,因此其深受化學工作者的青睞。由于石墨烯制備的催化劑不易回收,于是我們將石墨烯做成磁性材料,合成了新型磁性納米催化劑Fe3O4@GO@Mo。在室溫條件下雙氧水的乙醚溶液中,將其用于環(huán)氧化合物開環(huán)反應,得到β-羥基過氧化物,產(chǎn)率較高。催化劑通過外加磁鐵即可回收,且催化劑循環(huán)使用6次后其催化活性沒有降低。隨后,我們將新型磁性納米催化劑Fe_3O_4@GO@Mo用于螺環(huán)吲哚類衍生物的合成。這種催化劑對于合成各種取代基的螺環(huán)吲哚類衍生物具有不錯的催化效果。該反應由靛紅衍生物、丙二腈和4-(苯基氨基)呋喃-2(3H)-酮類衍生物三組分為原料,在低共熔溶劑(氯化膽堿:尿素=1:2)中,微波加熱的條件下反應,得到具有不同取代基的螺環(huán)吲哚類衍生物的終產(chǎn)物,收率較高。此方法以低共溶溶劑作為反應條件綠色無污染,并且溶劑可回收利用。我們還合成了新型磁性納米催化劑Fe_3O_4@GO@SO_3H,用于吡唑并[3,4-b]吡啶類衍生物的合成。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)丙腈為原料,在低共溶溶劑(氯化膽堿:甘油=1:3)中,催化劑Fe_3O_4@GO@SO_3H存在的條件下80℃得到終產(chǎn)物吡唑并[3,4-b]吡啶衍生物,收率較高。并且磁性納米材料的諸多優(yōu)點如:制備簡單、便于與產(chǎn)物分離和可循環(huán)利用等,都使得磁性納米材料廣泛應用于有機合成中成為可能。
[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，
本文編號：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，
本文編號：2307463
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