3,3′-二氯联苯胺的合成  

Synthesis of 3,3′-Dichlorobenzidine

作　　者：崔玉民[1] 范少华[1] 

机构地区：[1]阜阳师范学院化学系,安徽阜阳236032

出　　处：《精细化工》2001年第4期236-238,共3页Fine Chemicals

基　　金：安徽省教委自然科学基金资助项目! (99JL0 162 )&&

摘　　要：以邻硝基氯苯 (Ⅰ)为起始原料 ,经过三步化学反应合成 3,3′ 二氯联苯胺 (Ⅳ ) :Ⅰ在 0 .2g 1,4 萘醌催化下与CH2 O NaOH[m(NaOH)∶m(CH2 O) =0 .95∶1 0 0 ]在 5 6～ 5 7℃反应 7h ,得到 2 ,2′ 二氯氧化偶氮苯 (Ⅱ) ,产率 91.0 % ;Ⅱ在 0 .5gAl-Ni合金及 0 .3g 1,4 萘醌催化下与水合肼在 5 6～ 5 7℃反应 7.5h ,得到 2 ,2′ 二氯氢化偶氮苯 (Ⅲ) ,产率 97.0 % ;Ⅲ在盐酸中分别于 5℃反应 2h、于 10℃反应 11h、于 2 3～2 4℃反应 11h ,得到Ⅳ ,产率 96 .9%。Ⅳ的总产率可达 85 .5 % ,纯度w (Ⅳ) =97.7%Dichlorobenzidine(Ⅳ) was synthesized from o nitrochlorobenzene(Ⅰ) by three step reactions.2,2′ Dichloroazoxybenzene(Ⅱ) was obtained in 91.0% yield through reaction of Ⅰ with CH 2O/NaOH (mass ratio of NaOH∶CH 2O=0.95∶1.00) in the presence of 1,4 naphthoqinone(0.2 g) at 56-57 ℃ for 7 h.2,2′ Dichlorohydrazobenzene(Ⅲ) was gained in 97.0% yield through reaction of Ⅱ with N\-2H\-4·H\-2O in the presence of Al Ni alloy(0.5 g) and 1,4 naphthoqinone(0.3 g) at 56-57 ℃ for 7.5 h.Ⅳ was got in 96.9% yield from Ⅲ by reacting with HCl/H\-2O successively at 5 ℃ for 2 h,at 10 ℃ for 11 h and at 23-24 ℃ for 11 h.Total yield and purity of Ⅳ can reach 85.5% and 97.7% respectively.

关 键 词：3 3′-二氯联苯胺 邻硝基氯苯 1 4-萘醌 AI-Ni合金 

分 类 号：Q625.63[生物学—生物物理学]