张新慧,刘欣然,吴双双,雷跃凡,陈天云.化学通报,2016,79(6):575.
对硝基邻苯二乙醚合成技术研究
Study on the Synthesis of 1,2-Diethoxy-4-nitrobenzene
投稿时间:2015-10-27  修订日期:2015-12-28
DOI:
中文关键词:  对硝基邻苯二乙醚,邻苯二酚,相转移催化,混酸硝化
英文关键词:1,2-Diethoxy-4-nitrobenzene,1,2-benzenediol, phase  transfer catalysis, nitrification
基金项目:
作者单位E-mail
张新慧 合肥工业大学化学与化工学院 15056985332@163.com 
刘欣然 合肥工业大学化学与化工学院  
吴双双 合肥工业大学化学与化工学院  
雷跃凡 合肥工业大学化学与化工学院  
陈天云* 合肥工业大学化学与化工学院 t-y99@163.com 
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中文摘要:
      以聚乙二醇为相转移催化剂,邻苯二酚与溴乙烷为原料合成邻苯二乙醚,再经过冰醋酸和硝酸硝化得到对硝基邻苯二乙醚。研究了反应温度、反应时间、原料摩尔比和催化剂用量等对反应收率的影响,获得了合成邻苯二乙醚的较佳工艺条件,n(C6H4(0H)2):n(NaOH):n(C2H5Br)=1:2.6:2.4,反应温度80℃,反应时间4h,催化剂用量2g;该反应条件下邻苯二乙醚平均收率88%;混酸硝化条件下合成对硝基邻苯二乙醚的较佳工艺条件为n(C10H14O2):n(HNO3)=1:1.2,乙酸25ml,反应时间30min,反应温度20℃,该反应条件下对硝基邻苯二乙醚平均收率为99%。
英文摘要:
      1,2-Diethoxybenzene was synthesized with 1,2-Benzenediol and bromoethane and polyethylene glycol as phase transfer catalyst. Then 1,2-Diethoxy-4-nitrophathalic was synthesized with 1,2-Diethoxybenzene dealt with acetic acid and nitric acid by nitration. The effects of the reaction temperature, reaction time, molar ratio of raw materials and amount of the catalyst on the yield of product were investigated. The optimal reaction condition of 1,2-diethoxybenzene was molar ratio of 1,2-Benzenediol to sodium hydroxide to bromoethane 1:2.6:2.4, reaction temperature 80℃, reaction time 4 hours, catalyst 2g,The average yield of 1,2-diethoxybenzene was 88% . The optimal reaction condition of 4-nitrophathalic was molar ratio of 1,2-diethoxybenzene and nitric acid to 1:1.2, acetic acid 25ml, reaction time 30 minutes , reaction temperature 20℃. The average yield of 4-nitrophathalic was 99%.
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