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以邻苯二酚与溴乙烷为原料、聚乙二醇为相转移催化剂合成邻苯二乙醚,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优化工艺条件:n(C6H4(OH)2)∶n(NaO H)∶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%。
With catechol and ethyl bromide as raw materials, polyethylene glycol as phase-transfer catalyst for the synthesis of o-diethyl ether, and then through the acetic acid and nitric acid nitration to give p-nitrophenyl ether. The effects of reaction temperature, reaction time, molar ratio of raw materials and the amount of catalyst on the reaction yield were investigated. The optimal technological conditions were obtained as follows: n (C6H4 (OH) 2) (C2H5Br) = 1: 2.6: 2.4, the reaction temperature is 80 ℃, the reaction time is 4h and the amount of catalyst is 2g. The average yield of o-phenylethyl ether under the reaction conditions is 88%. The optimum conditions for the synthesis of p-nitrophenyldiethanolamide were as follows: n (C10H14O2): n (HNO3) = 1: 1.2, acetic acid 25mL, reaction time 30min and reaction temperature 20 ℃. The average yield of base o-phenylethyl ether was 99%.