| 微波辐射下无溶剂合成苯并咪唑-2-酮 |
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| 引用本文： | 吕维忠,刘波,韦少慧.微波辐射下无溶剂合成苯并咪唑-2-酮[J].精细石油化工,2006,23(4):4-6. |
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| 作者姓名： | 吕维忠 刘波 韦少慧 |
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| 作者单位： | 深圳大学理学院,广东,深圳,518060 |
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| 基金项目： | 深圳大学科研启动基金资助项目(200521)。 |
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| 摘 要： | 以多聚磷酸(PPA)为催化剂,邻苯二胺和脲为原料,在微波辐射下无溶剂合成了苯并咪唑-2-酮,反应时间由2～3 h缩短到6～10 min,产率为62．81％;正交实验所得影响因素顺序为:微波功率>照射时间>原料配比>催化剂用量。最优化合成工艺条件为:n(邻苯二胺):n(脲)为1:2;微波功率为126 W;反应时间为7 min;数字熔点仪、红外光谱(IR)与核磁共振谱(1H NMR)等测试结果表明产物为苯并咪唑-2-酮。
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| 关 键 词： | 微波照射 无溶剂 苯并咪唑-2-酮 邻苯二胺 脲 |
| 收稿时间： | 2005-10-10 |
| 修稿时间： | 2006-06-13 |
SOLVENT-FREE SYNTHESIS OF 2-KETONE BENZIMIDAOZOLE UNDER MICROWAVE IRRADIATION |
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| Lu Weizhong,Liu Bo,Wei Shaohui.SOLVENT-FREE SYNTHESIS OF 2-KETONE BENZIMIDAOZOLE UNDER MICROWAVE IRRADIATION[J].Speciality Petrochemicals,2006,23(4):4-6. |
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| Authors: | Lu Weizhong Liu Bo Wei Shaohui |
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| Affiliation: | College of Science, Shenzhen University, Shenzhen 518060, Guangdong , China |
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| Abstract: | 2-Ketone benzimidaozole was synthesized by the reaction of o-phenylenediamine and carbamide in the presence of polyphosphoric acid (PPA), under microwave irradiation and solvent-free conditions. This is a simple and inexpensive method for the synthesis of 2-ketone benzimidaozole. The reaction time of this new method is 6 - 10 min, much shorter than the 2 - 3 h in the traditional method, with the yield of 62. 81%. The results of orthogonally arranged experiments showed that the order of the effective factor is microwave power > radiation time> ratio of raw materials> concentration of catalyst. The optimal reaction conditions were found as follows: mol ratio of o-phenylendiamine/thiourea 1 : 2, microwave power 126 W, reaction time 7 min. The structure of the product was characterized by melting point determination, IR, 1H NMR, etc. |
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| Keywords: | microware irradiation solvent-free 2-ketone benzimidaozole o-phenylenediamine carbamide |
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