微波诱导催化交换氟化合成对氟硝基苯

Synthesis of p-Fluoronitrobenzene by Halogen-exchange under Microwave Irradiation

该文研究了微波辐射和常规加热下卤素交换氟化合成对氟硝基苯的方法 ,提出了共沸干燥和微波干燥制备无水KF的方法。结果表明 ,于微波辐射下 ,用微波干燥KF为氟化剂 ,在十六烷基三甲基溴化铵存在下于DMSO中反应 2 .5h可得 90 .2 %的产率 ,反应速率是常规加热的 2 .4倍 ,产率由 86 .8%提高到 90 .2 % ,以喷雾干燥KF为氟化剂 ,则产率可达 92 .2 %。

The halogen exchange method to prepare p fluoronitrobenzene under microwave irradiation and conventional heat was studied. Drying KF by azeotropy and microwave irradiation was proposed. The results showed that p fluoronitrobenzene was obtained by a yield of 90.2 % after reacting 2.5 h under microwave irradiation from a reaction system including microwave dried KF, cetyltrimethylammonium bromide and DMSO. The reaction rate was 2.4 times as high as that in traditional method, and the yield of p fluoronitrobenzene was also promoted from 86.8 % to 90.2 %. But the yield as high as 92.2 % could be obtained by using spray dried KF as fluorinating reagent.