5,6-二氨基苯并咪唑酮-2的合成  

Synthesis of 5,6-Diaminobenzimidazolone-2

作　　者：邵丹凤[1,2] 周国权[1,2] 杨泽慧[1] 陈新志[2] 

机构地区：[1]宁波工程学院化工学院,浙江宁波315016 [2]浙江大学化学工程与生物工程学系,浙江杭州310027

出　　处：《精细化工》2010年第5期500-503,520,共5页Fine Chemicals

基　　金：宁波市石油化工人才培养基地项目(No.Jd080135);宁波工程学院项目(No.2007029)~~

摘　　要：以苯并咪唑酮-2为原料,经混酸硝化、催化加氢还原合成5,6-二氨基苯并咪唑酮-2,总收率62.1%。用单因素法优化了工艺条件,硝化反应:n(硝酸)/n(苯并咪唑酮-2)=2.2,0℃反应6 h,5,6-二硝基苯并咪唑酮-2收率为69%;催化加氢还原反应:m(Raney-Ni)/m(5,6-二硝基苯并咪唑酮-2)=0.09,于100℃、2.5 MPa下无水乙醇中反应9 h,5,6-二氨基苯并咪唑酮-2收率90%。中间体和目标产物用MS、HPLC、IR、1HNMR、13CNMR和元素分析等方法分析,确认其结构。5,6-Diaminobenzimidazolone-2 is obtained in an overall yield of 62.1% by the nitration of benzimidazolone-2 and followed with hydrogenation.Single-factor experiments were conducted to optimize the reaction condition.5,6-Dinitrobenzimidazolone-2 was synthesized by the nitration of benzimidazolone-2 under 0 ℃,for 6 h,n（nitric acid）/n（benzimidazolone-2）=2.2 in 69% yield.5,6-Diaminobenzimidazolone-2 was prepared in the absolute alcohol in 90% yield by 9 h of the Raney-Ni catalytic hydrogenation of 5,6-dinitrobenzimidazolone-2 under the condition of 100 ℃、2.5 MPa、m（catalyst）/m（5,6-dinitrobenzimidazolone-2）=0.09.MS、HPLC、IR、1HNMR、13CNMR and elementary analysis are properly used for the characterization of the structures of the product.

关 键 词：5 6-二氨基苯并咪唑酮-2 苯并咪唑酮-2 5 6-二硝基苯并咪唑酮-2 选择性硝化 催化加氢 精细化工中间体 

分 类 号：O626.23[理学—有机化学]