摘要
研究了二硝基苯类化合物的氟代脱硝反应,考察了溶剂和氟化剂的种类与用量、反应时间、催化剂等因素对反应的影响。结果表明,在二硝基苯用量为2.1 g（12.5 mmol）、喷雾干燥无水氟化钾用量为2.9 g（50 mmol）、四苯基溴化鏻用量为0.53 g（1.25 mmol）、四乙二醇二甲醚用量为0.13 mL（0.625 mmol）、NO2-捕捉剂邻苯二甲酰氯用量为1.8 mL（12.5 mmol）的优化投料条件下,以硝基苯为反应介质,反应温度210℃,反应时间1~5 h,原料转化率高达94.1%~98.5%,硝基氟苯收率可达81.6%~87.4%。
Fluorodenitration is one of the efficient methods for preparation of fluoronitrobenzenes with the advantages of raw material availability, simple process, and high product yields. In this paper, fluorodenitration of dinitrobenzenes was studied. The effects of fluorinating agent, solvent, reaction time, and catalyst, etc on the fluorodenitration were studied. The results show the optimum reaction conditions were 2. 1 g（ 12. 5 mmol） of dinitrobenzene, 2. 9 g（50 mmol） of SD-KF, 0. 53 g（1.25 mmol） of Ph4PBr, 0. 13 mL（2. 5 mmol） of tetraethylene glycol dimethyl ether in the presence of 1.8 mL（ 12. 5 mmol） of PDC as a trapping agent of NO2-, and the mixture was stirred at 210℃ for 1 -5 h in nitrobenzene, resulting in 94. 1% -98. 5% conversions and 81.6% ~ 87. 4% yields.
出处
《应用化学》
CAS
CSCD
北大核心
2008年第11期1356-1360,共5页
Chinese Journal of Applied Chemistry
关键词
二硝基苯
硝基氟苯
氟代脱硝
相转移催化
dinitrobenzenes, fluoronitrobenzenes ,fluorodenitration,phase transfer catalysis
