新型微通道反应器中合成2-羟基-3-三氟甲基-5-硝基吡啶  

SYNTHESIS OF 2-HYDROXY-3-TRIFLUOROMETHYL-5-NITROPYRIDINE BY THE MICRO-CHANNEL REACTOR

作　　者：陈玉娴 赵转霞 刘耀赟 Chen Yuxian;Zhao Zhuanxia;Liu Yaoyun(Gansu Andrews Fortune Pharmaceutical Co.,Ltd.,Lanzhou 730300,Gansu,China)

机构地区：[1]甘肃安卓幸制药有限公司,甘肃兰州730300

出　　处：《精细石油化工》2022年第5期39-42,共4页Speciality Petrochemicals

摘　　要：采用新型微通道设备,以2-羟基-3-三氟甲基吡啶为原料制备了2-羟基-3-三氟甲基-5-硝基吡啶,并用高效液相色谱仪表征反应进程及反应产物成分。在最佳反应条件下,n(硝酸)∶n(原料)=2.10∶1、温度90℃、停留时间40.0 s、混合酸强91.15%;后处理中和剂为25%氨水、中和后pH为5~6,最终产物收率可提高至63%~65%。A micro-channel reactor was used to prepare 2-hydroxy-3-trifluoromethyl-5-nitropyridine from 2-hydroxy-3-trifluoromethylpyridine.Meanwhile,the reaction process and product components were characterized by high performance liquid chromatography(HPLC).Finally,the yield is increased to 63%-65%,and the optimal reaction conditions are as follows:n(HNO)∶n(material)=2.10∶1,temperature 90℃,residence time 40.0 s,mixed acid strength 91.15%.Post treatment conditions are as follows:the neutralizing agent is 25%ammonia water,and the pH value after neutralization is 5-6.

关 键 词：2-羟基-3-三氟甲基-5-硝基吡啶 新型微通道设备 硝化反应 

分 类 号：O62[理学—有机化学] O69[理学—化学]