引用本文:
胡玉锋, 罗军, 梁政勇, 黄成美, 吕春绪. 氟代脱硝制备含氟硝基苯[J]. 应用化学,
2008, 25(11): 1356-1360.
Citation: HU Yu-Feng, LUO Juna, LIANG Zheng-Yong, HUANG Cheng-Mei, LV Chun-Xu. Synthesis of Fluoronitrobenzenes by Fluorodenitration[J]. Chinese Journal of Applied Chemistry, 2008, 25(11): 1356-1360.
Citation: HU Yu-Feng, LUO Juna, LIANG Zheng-Yong, HUANG Cheng-Mei, LV Chun-Xu. Synthesis of Fluoronitrobenzenes by Fluorodenitration[J]. Chinese Journal of Applied Chemistry, 2008, 25(11): 1356-1360.
氟代脱硝制备含氟硝基苯
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%。
English
Synthesis of Fluoronitrobenzenes by Fluorodenitration
Abstract:
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.
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Key words:
- dinitrobenzenes
- / fluoronitrobenzenes
- / fluorodenitration
- / phase transfer catalysis
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