1,2,3-三氟-4-硝基苯的合成  

Synthesis of 1,2,3-Trifluoro-4-Nitrobenzene

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：《石油化工》2002年第7期555-557,共3页Petrochemical Technology

基　　金：安徽省教委自然科学基金资助项目 ( 2 0 0 1KJ184)

摘　　要：以 2 ,6 -二氯苯胺 (A)为起始原料 ,经 4步化学反应合成了 1,2 ,3-三氟 -4 -硝基苯。A于 0～ 5℃分别与NaNO2 /HCl、HBF4反应 ,得到 2 ,6 -二氯苯氟硼酸重氮盐 (B) ,产率 88.8%;B在 15 5℃分解 ,生成 2 ,6 -二氯氟苯(C) ,产率 91.5 %;C在无水Na2 SO4作用下与HNO3 /H2 SO4在 15℃反应 90min .,得到 2 ,6 -二氯 -3-硝基氟苯(D) ,产率 95 .1%;D在 18-冠 -6的催化下与氟化钾在 15 0℃反应 12h ,得到 1,2 ,3-三氟 -4 -硝基苯 (E) ,平均产率 6 2 .0 %。E的总收率达到 47.9%,纯度为 99.0 %。trifluoro-4-nitrobenzene(E) was synthesized from 2,6-dichloroaniline(A) through the following four chemical reaction steps: 2,6-dichlorophenyl-diazonium borofluoride complex(B) was obtained with 88.8% yield through A by reaction with NaNO 2/HCl and HBF 4 at 0～5 ℃,respectively; 2,6-dichloro-fluorobenzene(C) was obtained with 91.5% yield through B by decomposition at 155 ℃;2,6-dichloro-3- nitro-fluorobenzene(D) was obtained with 95.1% yield through C by reaction with HNO 3/H 2SO 4 in the presence of anhydrous Na 2SO 4 at 15 ℃ for 90 min,and finally E was produced with 62.0% yield through D by reaction with KF in the presence of 18-crown-6 at 150 ℃ for 12 h with repeated use of the mother liquor.The total yield and the purity of E reach 47.9% and 99.0%,respectively.

关 键 词：1 2 3-三氟-4-硝基苯 合成 2 6-二氟苯胺 2 6-二氯氟苯 

分 类 号：TQ246.12[化学工程—有机化工]