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作 者:蒋锐[1] 董燕敏[1] 杨金会[2] 赵天生[2] 陈兴权[1]
机构地区:[1]常州大学石油化工学院,江苏常州213164 [2]宁夏大学能源化工重点实验室,宁夏银川750021
出 处:《精细石油化工》2013年第1期12-16,共5页Speciality Petrochemicals
基 金:国家自然科学基金(20962016)
摘 要:以4-氟苯胺为原料,经乙酰化、氯代、水解、重氮化-桑德迈耳以及硝化合成了2-氟-4,5-二氯硝基苯。乙酸酐为乙酰化试剂合成4-氟乙酰苯胺,收率为95.9%;4-氟乙酰苯胺再经SO2Cl2氯代反应,合成2-氯-4-氟乙酰苯胺,收率为79.1%;2-氯-4-氟乙酰苯胺水解合成2-氯-4-氟苯胺,收率为73.6%;2-氯-4-氟苯胺经重氮化氯代制得3,4-二氯氟苯,收率为48.0%;3,4-二氯氟苯经硝化制得目的产物2-氟-4,5-二氯硝基苯,收率74.9%。过程的总收率为20.1%。4,5-Dichloro-2-fluoronitrobenzene was prepared from 4-fluoroaniline through a route, name- ly acetylation, chlorination, hydrolysis, diazotization-Sandmeyer, and then nitrification. Firstly, 4- fluoroaniline reacted with acetic anhydride. The yield of the obtained 4-fluoroacetanilide reached 95.9%. 4-Fluoroacetanilide converted to 2-chloro-4-fluoroacetaniline through sulfuryl chloride. The yield of the obtained 2-chloro-4-fluoroacetaniline was 79. 1%. 2-Chloro-4-fluoroaniline could be pre- pared from 2-chloro-4-fluoroacetaniline with the yield of 73.6%, 3,4-Dichlorofluorobenzene was pre- pared by diazotization-Sandmeyer with the yield of 48.0%. Finally, 4,5-dichloro-2-fluoronitrobenzene was prepared by nitrification with the yield of 74.9 %. The total yield of 4,5-dichloro-2-fluoronitro- benzene by this route was 20.1 G.
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