超声波强化2,3,4-三氟硝基苯的合成  

Ultrasonic Promoted in Synthesis of 2,3,4-trichloronitrobenzene

作　　者：陆云强[1] 陈国辉[1] 

机构地区：[1]中南大学化学化工学院,湖南长沙410083

出　　处：《广东化工》2009年第3期20-22,共3页Guangdong Chemical Industry

摘　　要：2,3,4-三氟硝基苯是重要的医药中间体,是合成第三代喹诺酮类抗菌药的起始原料。文章以1,2,3-三氯苯为原料,与HNO3/H2SO4反应制得2,3,4-三氯硝基苯,再在超声波辐射下,以四甲基氯化铵为催化剂,DMSO为溶剂,与KF制得2,3,4-三氟硝基苯。考察了超声波辐射时间、功率以及其它反应条件对反应过程的影响。得到了优化合成工艺条件:HNO3/1,2,3-三氯苯的摩尔比为1.3︰1,反应温度55～60℃。超声波反应时间20 min,功率25%,模式:间歇式脉冲2 min;该合成方法有效减少了合成步骤,提高了合成效率,具有工业化前景。2,3,4-trifluoronitrobenzene is an important pharmaceutical intermediate, mainly been used as the starting material to synthesis the third generation quinolones antibacterial drugs such as lomefloxaxin, ofloxacin etc. The 1,2,3-trichlorobenzene was used as the raw material in the paper, reacted with HNO3/H2SO4 to prepare 2,3,4 - trichloronitrobenene at first, then catalyzed by tetra-methyl ammonium chloride react with KF in DMSO in the present of ultrasonic waves to give 2,3,4-trifluoronitrobenzene. Considered the reaction conditions impacting on the nitration and fluorination, the optimal condition were found： the molar ratio HNO3/1,2,3-trichlorobenzene： 1.3 ： 1, the reaction temperature： 55-60℃. Ultrasonic reaction time： 20 min, power： 25 %, Ultrasonic mode： intermittent pulse 2 second; which could effectively reduce the synthesis steps, with great prospect of industrialization.

关 键 词：1 2 3-三氯苯 硝化 氟取代 超声波辐射 

分 类 号：TQ625[化学工程—精细化工]