间三氟甲基苯胺合成尼鲁米特  

A New Method for the Synthesis of Nilutamide by m-Trifluoromethylaniline

作　　者：陶晓红[1] 张文城[1] 石勇[1] 吴振刚[1] 谢艳[1] 

机构地区：[1]衢州学院,浙江衢州324000

出　　处：《化工生产与技术》2014年第5期9-11,7,共3页Chemical Production and Technology

基　　金：浙江省教育厅项目资助项目;衢州学院大学生科技创新项目资助(Q12X31;Q13X08)

摘　　要：以间三氟甲基苯胺为原料,经重氮化碘代、硝基化、缩合反应合成尼鲁米特,考察了摩尔配比、硝酸浓度、催化剂的选择对各反应的影响。结果表明,优化的反应条件分别是:重氮化碘代反应,反应温度10℃,间三氟甲基苯胺与盐酸摩尔比为1:3.5;硝化反应,反应温度10℃,硝酸的质量分数为90%,间碘三氟甲苯与硝酸的摩尔配比为1:1.3;缩合反应以CuCl为催化剂。总收率约为35%。其结构经熔点、核磁共振、质谱验证无误。该工艺反应路线较短、条件温和、收率高、原料价廉易得,适合工业化生产。Using m-trifluoromethylaniline as raw material,through diazotization iodo-substitution,nitration and condensation reaction for the synthesis of Nilutamide.An optimized process was obtained by investigating the influence of reaction molar ratios,the concentration of HNO_3 and the selection of catalysts on the product yield:the diazotization iodo-substitution reaction temperature was10℃,the molar ratio of m-trifluoromethylaniline and hydrochloric acid was 1:3.5;the nitration reaction temperature was 10℃,the mass fraction of nitric acid was 90%,the molar ratio of m-trifluoromethylaniline and nitric acid was 1:1.3;the condensation reaction catalyst was CuCl,the total yield was 35%.The chemical structure was confirmed by means of ~1H-NMR,MS and m.p.data.The advantages of the synthesis are short reaction course,mild conditions,high yield and cheapness raw material.It is suitable for industrialized production.

关 键 词：尼鲁米特 合成 间三氟甲基苯胺 

分 类 号：TQ467[化学工程—制药化工]