以富勒烯和乙二胺为原料合成富勒烯乙二胺,富勒烯乙二胺再与硝酸铅反应得到富勒烯乙二胺铅盐。通过单因素方法探讨了反应物物料比、反应温度以及反应时间对富勒烯乙二胺铅盐中铅含量的影响,获得最佳工艺条件为:富勒烯乙二胺和硝酸铅的...以富勒烯和乙二胺为原料合成富勒烯乙二胺,富勒烯乙二胺再与硝酸铅反应得到富勒烯乙二胺铅盐。通过单因素方法探讨了反应物物料比、反应温度以及反应时间对富勒烯乙二胺铅盐中铅含量的影响,获得最佳工艺条件为:富勒烯乙二胺和硝酸铅的摩尔比为1∶15,反应时间为2.0h,反应温度为35℃,所得富勒烯乙二胺铅盐中铅含量为49.4%。同时采用FT-IR、1 H NMR、XPS及AAS等测试手段对产物结构进行了表征。采用差热和热重分析法对富勒烯乙二胺铅盐的热稳定性进行了研究,结果表明,在空气气氛下,分解峰值温度为310℃,表明产物热稳定性良好。展开更多
Transition-metal-salt-mediated radical reactions of fullerenes have attracted extensive attention as a new and important method for fullerene functionalization. The application of relatively cheap and easily available...Transition-metal-salt-mediated radical reactions of fullerenes have attracted extensive attention as a new and important method for fullerene functionalization. The application of relatively cheap and easily available ferric perchlorate (Fe(ClO 4 ) 3 ) to the synthesis of [60]fullerene (C 60 ) has demonstrated remarkable advantages and afforded a series of novel fullerene derivatives. In this review we present our recent progress in this area and summarize the reactions of C 60 with malonate esters, β-keto esters, nitriles, aldehydes/ketones, and arylboronic acids in the presence of Fe(ClO 4 ) 3 to afford the C 60-fused disubstituted lactones, C 60-fused hemiketal, C 60-fused dihydrofuran, C 60-fused oxazoles, C 60-fused 1,3-dioxolanes, and fullerenyl boronic esters. The possible reaction mechanisms for the above-mentioned reactions are also described in detail.展开更多
文摘以富勒烯和乙二胺为原料合成富勒烯乙二胺,富勒烯乙二胺再与硝酸铅反应得到富勒烯乙二胺铅盐。通过单因素方法探讨了反应物物料比、反应温度以及反应时间对富勒烯乙二胺铅盐中铅含量的影响,获得最佳工艺条件为:富勒烯乙二胺和硝酸铅的摩尔比为1∶15,反应时间为2.0h,反应温度为35℃,所得富勒烯乙二胺铅盐中铅含量为49.4%。同时采用FT-IR、1 H NMR、XPS及AAS等测试手段对产物结构进行了表征。采用差热和热重分析法对富勒烯乙二胺铅盐的热稳定性进行了研究,结果表明,在空气气氛下,分解峰值温度为310℃,表明产物热稳定性良好。
基金supported by the National Natural Science Foundation of China (20972145, 21132007, 21102041)National Basic Research Program of China (2011CB921402)Scientific Research Foundation of Education Commission of Hubei Province (Q20120113)
文摘Transition-metal-salt-mediated radical reactions of fullerenes have attracted extensive attention as a new and important method for fullerene functionalization. The application of relatively cheap and easily available ferric perchlorate (Fe(ClO 4 ) 3 ) to the synthesis of [60]fullerene (C 60 ) has demonstrated remarkable advantages and afforded a series of novel fullerene derivatives. In this review we present our recent progress in this area and summarize the reactions of C 60 with malonate esters, β-keto esters, nitriles, aldehydes/ketones, and arylboronic acids in the presence of Fe(ClO 4 ) 3 to afford the C 60-fused disubstituted lactones, C 60-fused hemiketal, C 60-fused dihydrofuran, C 60-fused oxazoles, C 60-fused 1,3-dioxolanes, and fullerenyl boronic esters. The possible reaction mechanisms for the above-mentioned reactions are also described in detail.
