相转移催化合成2,4-二硝基氟苯的研究

以2,4-二硝基氯苯为原料,采用相转移催化合成了2,4-二硝基氟苯。考察了不同摩尔比、温度、反应时间、相转移催化剂、氟化钾的干燥方式、水量对反应的影响。结果表明,四甲基氯化铵为最优催化剂,通过喷雾干燥的KF活性最高,反应体系的水分控制在0.2%为最佳,在投料比为n(2,4-二硝基氯苯)∶n(KF)∶n(催化剂)=1∶1.1∶0.01,回流状态下反应6h,氟代产物的收率为95.1%。

Synthesis of 2,4-Dinitrofluorobenzene by Phase Transfer Catalysis

2,4-Dinitrofluorobenzene was synthesized by using 2,4-dinitrochlorobenzene as the starting material via phase transfer catalysis.The influencing factors of the reaction,such as mole ratio,reaction temperature,reaction time,catalyst,potassium fluoride and amount of water were investigated.The optimal conditions were obtained.The results showed that tetramethylammonium chloride was the optimum catalyst,and the reaction was conducted using spray dried potassium fluoride containing less than 0.2% water at the ratio of n(2,4-dinitrochlorobenzene)∶n(KF)∶n(catalyst) =1∶1.1∶0.01.After reacting with reflux for 6 h,the yield was 95.1%.