摘要
以壳聚糖为原料,在乙醇溶液中通过将其与2-吡啶甲醛反应制得Schiff碱功能化的壳聚糖(PYCS),然后将PYCS与Cu Br进行络合反应制得负载型催化剂(PYCS-Cu Br).采用红外光谱、热重分析和X射线衍射分析等方法对PYCS-Cu Br催化剂进行表征.热重分析结果表明,该催化剂在200℃以内具有较好的热稳定性,能够满足其使用温度.结合微波辐射技术以及"一锅法"合成策略,以PYCS-Cu Br为催化剂催化有机炔、卤代烷以及Na N3之间的环加成反应.结果表明,PYCS-Cu Br催化剂具有良好的催化性能,在微波辐射功率为480 W,温度为70℃条件下,15 min可快速制得1,2,3-三唑类化合物,该催化剂易回收,且可重复使用至少4次,活性未见明显降低.放大反应结果表明,1,2,3-三唑类化合物能够以较高收率并以数十克规模制备.
Pyridine-2-carboxaldehyde-modified chitosan（ PYCS） was prepared through a simple procedure using chitosan（ CS） and pyridine-2-carboxaldehyde in ethanol solution. Subsequently,PYCS supported CuBr（ PYCS-CuBr） was synthesized by the reaction of PYCS with CuBr in acetone at room temperature under N2 atmosphere. The obtained catalyst was characterized by FTIR,TGA and XRD. TGA result showed that the catalyst had a good stability up to 200 ℃ and could meet the normal use. The catalytic performances were evaluated in one-pot multi-component copper（ Ⅰ）-catalyzed azide-alkyne cycloaddition（ Cu AAC） reaction under microwave-assisted condition. PYCS-CuBr was found to exhibit obvious catalytic activity to rapidly produce 1,2,3-triazole compounds under the microwave irradiation（ 480 W） at 70 ℃. Furthermore,the catalyst could be easily recovered by simple filtration and recycled at least 4 cycles without obvious loss of catalytic activity. 1,2,3-triazoles can be exclusively generated on multi-gram scale.
作者
熊兴泉
江云兵
肖上运
石霖
宋思达
XIONG Xingquan JIANG Yunbing XIAO Shangyun SHI Lin SONG Sida(College of Materials Science and Engineering, Huaqiao University, the Key Laboratory for Functional Materials of Fujian Higher Education, Xiamen 361021, China)
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2016年第10期1863-1869,共7页
Chemical Journal of Chinese Universities
基金
国家自然科学基金(批准号:21004024)
福建省自然科学基金(批准号:2016J01063)
福建省“高校新世纪优秀人才支持计划”(批准号:2012FJ-NCET-ZR03)
“华侨大学中青年教师科研提升资助计划”(批准号:ZQN-YX103)资助~~
