钯催化氰基化反应合成对氰基苯甲酸
Synthesis of 4-cyanobenzoic acid by palladium catalyzed cyanation reaction
作者：付磊清;李小港;康艳萍;郭孟萍;
Author：
收稿日期： 年卷（期）页码：2015,30(05):-528-530
期刊名称：华西药学杂志
Journal Name：WEST CHINA JOURNAL OF PHARMACEUTICAL SCIENCES
关键字：对氰基苯甲酸;亚铁氰化钾;钯配合物催化剂;氰基化反应;合成;条件优化
Key words：
基金项目：国家自然科学基金资助项目(批准号:21063015)
中文摘要
目的合成对氰基苯甲酸,并考察其催化反应条件。方法以对溴苯甲酸为原料、K4Fe(CN)6·3H2O为氰基化试剂、双(O-二苯基膦苯甲酸)钯配合物[(O-Ph2PC6H4COO)2Pd]为催化剂,经溴代芳烃的氰基化反应合成对氰基苯甲酸;考察K4Fe(CN)6·3H2O、钯配合物和K3PO4的用量、温度、时间和溶剂等对反应的影响。结果目标产物的化学结构经1HNMR、13CNMR确证,收率为82.3%,HPLC纯度>94.6%。最佳反应条件为:对溴苯甲酸、K4Fe(CN)6·3H2O、(O-Ph2PC6H4COO)2Pd及K3PO4的比例为1.0∶0.3∶0.02∶2.0,溶剂为N,N-二甲基甲酰胺,温度为125~130℃,时间12 h。结论所用方法具有原料易得、条件温和、操作简便、收率高等优点。
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