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作 者:高秋敏 严明 周飞翔 张巍伟 冯吉玉 张晓阳 GAO Qiu-min;YAN Ming;ZHOU Fei-xiang;ZHANG Wei-wei;FENG Ji-yu;ZHANG Xiao-yang(Jiangsu Ruixiang Chemical Co.,Ltd.,Jiangsu Yangzhou 225000,China)
出 处:《广州化工》2022年第5期97-100,共4页GuangZhou Chemical Industry
摘 要:通过筛选一系列NHC配体催化剂,构建以氨气为氨源对邻氯甲苯进行胺化合成邻甲苯胺的催化体系。考察溶剂和反应条件对邻氯甲苯转化率和选择性的影响,并优化了反应条件。采用核磁共振波谱仪对催化剂进行表征,用气相色谱(GC)对产物进行定量分析,气质联用(GC-MS)进行定性分析。结果表明,NHC-CuCl为较好的催化剂,1,4-二氧六环是适合的溶剂,叔丁醇钾是不错的脱酸剂,180℃下反应8 h后,邻氯甲苯的转化率为71.9%,选择性为62.2%。A catalytic system for the synthesis of o-toluidine from o-chlorotoluene amination with ammonia was fabricated by screening a series of catalysts. The effects of solvents and reaction conditions on o-chlorotoluene conversion and o-toluidine selectivity were investigated, and the reaction conditions were optimized. The catalyst were characterized by using NMR,and the reacting products were analyzed by GC and GC-MS for quantitative and qualitative analysis, respectively. The results showed that NHC-CuCl was a good catalyst and 1,4-dioxaneis was a suitable solvent, and potassium tert-butoxide was a suitable deacidification agent for this reaction. Under the optimal reaction conditions of 180 ℃ for 8 h, 71.9% conversion of o-chlorotoluene with 62.2% of o-toluidine selectivity were obtained.
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