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。
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： tool 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.
出处
《精细石油化工》
CAS
CSCD
北大核心
2006年第4期4-6,共3页
Speciality Petrochemicals
基金
深圳大学科研启动基金资助项目(200521)。
关键词
微波照射
无溶剂
苯并咪唑-2-酮
邻苯二胺
脲
microware irradiation
solvent-free
2-ketone benzimidaozole
o-phenylenediamine
carbamide
