3-甲氧基二苯胺的合成新工艺

A Novel Synthetic Process of 3-Methoxy Diphenylamine

建立了3-甲氧基二苯胺的合成新工艺。以易得、价廉的间二硝基苯为原料,经取代、加氢还原、缩合脱水三步反应制备3-甲氧基二苯胺。确定适宜的缩合脱水反应条件为:以磷酸芳基酯为催化剂、反应原料苯酚和3-甲氧基苯胺的物质的量比为1.2∶1、反应温度为90℃、反应时间为10h,在该条件下,缩合脱水反应收率为86.7%,总收率达到69.9%(以间二硝基苯计)。该工艺优于经典的乌尔曼合成路线,生产成本大大降低,具有很好的工业化前景。

A novel synthetic process of 3-methoxy diphenylamine had been established.With easy and inex-pensive m-dinitrobenzene as raw material,3-methoxy diphenylamine was prepared by three-step reaction of sub-stitution,hydrogenation reduction and condensation dehydration.The optimum reaction conditions of condensation dehydration were determined as follows：with aryl phosphate ester as catalyst,the molar ratio of phenol and 3-methoxy phenylamine was 1.2∶1,reaction temperature was 90 ℃,reaction time was 10 h.Under above conditions,the yield of the condensation dehydration was 86.7% and the total yield was 69.9%（on the basis of mdinitrobenzene）.The novel process is superior to the classic Ullmann synthetic route,greatly reduces the production cost and has good industrial prospect.