4,6-二乙氧基间苯二胺的合成

以1,5-二氯-2,4-二硝基苯（DCDNB）为原料，经烷氧基化和催化加氢还原反应合成4,6-二乙氧基间苯二胺（DEDAB），并探索了其影响因素。结果表明合成中间体1,5-二乙氧基-2,4-二硝基苯（DEDNB）的较佳条件为：n(DCDNB)∶n(NaOH)∶n(无水C2H5OH)=1∶4∶30，室温下反应7 h，收率96.43%，HPLC纯度99.74%；产品DEDAB的较优合成工艺条件为：n(DEDNB)∶n(无水C2H5OH)= 1∶44，w(10%Pd/C)/w(DEDNB)= 10%，反应时间7 h，反应温度110 ℃，氢气压力1.5 MPa，收率95.42%，HPLC纯度98.87%。产品及中间体结构经1H NMR、MS 和FTIR分析表征确认。

Synthesis of 4,6-diethoxy phenylenediamine

Through alkoxylation and catalytic hydrogenation reduction reaction,4,6-diethoxy phenylenediamine(DEDAB)was synthesized from 1,5-dichloro-2,4-dinitrobenzene(DCDNB)and the experimental conditions,such as materials ratio,reaction temperature and reaction time,were investigated.Proper experimental condition for alkoxylation reaction were found as:n(1,5-dichloro-2,4-dinitrobenzene)∶n(NaOH)∶n(anhydrous C2H5OH)= 1∶4∶30,room temperature,reaction time 7 h,under which the yield of 1,5-diethoxy-2,4-dinitrobenzene(DEDNB) was 96.43% based on DCDNB and the purity was 99.74% as determined by HPLC;proper catalytic hydrogenation reduction reaction conditions were found as:n(1,5-diethoxy-2,4-dinitrobenzene)∶n(anhydrous C2H5OH)= 1∶44,w(10% Pd/C)∶w(DEDNB)=10%,reaction temperature 110 ℃,reaction time 7 h,pressure of hydrogen 1.5 MPa,under which the yield of DEDAB was 95.42% based on DEDNB and the purity was 98.87% as determined by HPLC.The molecular structures of product and its intermediates were identified by 1H NMR,MS and FTIR.