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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。
Benzimidazolone-2 was used as raw material to synthesize 5,6-diaminobenzimidazolone-2 by mixed acid nitration and catalytic hydrogenation to reduce the total yield to 62.1%. The process conditions were optimized by single factor method. The nitration reaction was: reaction of n (benzimidazolone-2) = 2.2 at 0 ℃ for 6 h, yield of 5,6-dinitrobenzimidazolone-2 Was 69%. The catalytic hydrogenation reduction reaction was: Raney-Ni / m (5,6-dinitrobenzimidazolone-2) = 0.09. The reaction was carried out in absolute ethanol at 100 ℃ and 2.5 MPa for 9 h , 5,6-diamino benzimidazolone-2 yield of 90%. The intermediate and the target product were analyzed by MS, HPLC, IR, 1HNMR, 13CNMR and elemental analysis to confirm the structure.