2,3,4-三氟硝基苯的合成  

Synthesis of 2,3,4-Trifluoronitrobenzene

作　　者：刘丽娜[1] 

机构地区：[1]安徽华源生物药业有限公司质检处,安徽阜阳236018

出　　处：《阜阳师范学院学报（自然科学版）》2001年第3期22-26,共5页Journal of Fuyang Normal University(Natural Science)

摘　　要：以2,6-二氯苯胺(A)为起始原料,经四步化学反应合成了2,3,4-三氟硝基苯。A于0～5℃分别与NaNO_2/HCl、HBF_4反应,得到2,6-二氯苯氟硼酸重氮盐(B),产率88.8％;B在155℃分解,生成2,6-二氯氟苯(C),产率91.5％;C在无水Na_2SO_4作用下与HNO_3/H_2SO_4在15℃反应90min,得到2,6-二氯-3-硝基氟苯(D),产率91.5％;D在18-冠-6的催化下与氟化钾在150℃反应12h,重复套用母液,得到2,3,4-三氟硝基苯(E),平均产率62.0％。标题化合物E原总收率达到47.9％,纯度为99.0％。2, 3, 4-Trifluoronitrobenzene(E) was synthesized from 2,6-dichloroaniline(A) by four chemical reactions: 2, 6-dichlorophenyl-diazonium borofluoride complex(B) was obtained in 88.8％ yield through A reacted with NaNO_2/HCl, HBF_4 at0～5℃, respectively, 2, 6-dichloro-fluorobenzene(C) was gained in 91.5% yield through B decomposed at 155℃, 2, 6-dichloro-3-nitro-fluorobenzene(D) was got in 95. 1% yield through C reacted with HNO_3/H_2SO_4 in the presence of anhydrous Na_2SO_4 at 15℃ for 90 min., and E was produced in 62.0％ yield through D reacted with KF in the presence of 18-crown-6 at 150℃ for 12h and mother liquor used repeatedly. The total yield and the purity of E can reach 47.9% and 99.0%, respectively.

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

分 类 号：O613[理学—无机化学]