2-硝基苯酚-4-磺酰胺的合成  

Synthesis of 2-Nitrophenol-4-Sulfonylamide

作　　者：李燕芸[1] 尹振晏[1] 胡应喜[1] 刘霞[1] 陈赤阳[1] 刘彬[1] 

机构地区：[1]北京石油化工学院化工系,北京102600

出　　处：《石油化工高等学校学报》2001年第3期10-13,共4页Journal of Petrochemical Universities

摘　　要：以邻氯硝基苯为原料 ,经氯磺化、氨解、水解酸化三步反应制备了 2 -硝基苯酚 -4 -磺酰胺。研究了各步反应的影响因素 ,在传统工艺的基础上优化了反应条件 ,最优反应条件是 :n(邻氯硝基苯 )∶n(氯磺酸 ) =1∶4 ,分次投料 ,并加入一定量的无水硫酸钠 ,反应温度为 1 4 0℃ ,反应时间为 6～ 7h ;将所得产品按n( 2 -硝基氯苯 -4 -磺酰氯 )∶n(氨水 ) =1∶1 .5加入氨水中 ,反应温度为 38～ 4 0℃ ,低温反应 2h ;最后于 30 %氢氧化钠溶液中水解 ,反应温度 1 0 0～ 1 0 5℃ ,反应时间为 3～ 4h ,并加入相转移催化剂 ,最后进行酸化 ,抽滤后得目标产品。总收率由 5 0 %提高为 70 % 。2-Nitrophenol-4-sulfonylamide was synthesized by sulfochlorination, ammoniation, hydrolysis from o - nitrochlorobenzene being as raw materials. The reaction conditions were optimized in material proportion, reaction temperature, reaction time. The optimum technological conditions were obtained as the follows: The molar ratio of n(o - C6ClH4NO2):n(HSO3Cl)=1:4; The raw material has been fed in batches and the ration Na2SO4 is added, reaction temperature is 140 °C, reaction time is 6 [similar to] 7 h. The product n(2-nitrochlorobenzene-4-sulfochlorides):n (NH3)=1:1.5 has been treated with ammonia water at reaction temperature 38 [similar to] 40 °C for 2 h, and treated with 30% NaOH solution at 105 °C for 3 [similar to] 4 h, and then phase transfer catalyst is added, finally after acidifying, the product can be obtained. The excellent yield was 70%. The three products obtained in above three phases were characterized by IR.

关 键 词：染料 中间体 氯磺化 氨解 水解酸化 邻氯硝基苯 合成 磺酰胺 硝基苯酚 

分 类 号：TQ612.6[化学工程—精细化工]