doi:10.16597/j.cnki.issn.1002-154x.2023.02.007
紫外吸收剂 UV - 1164 的工艺开发
姬金岭 孙立娇 黄姗珊 赵慧 史成阳 王运良∗
(佳木斯大学 药学院, 黑龙江 佳木斯 154007)
Development and Industrialization of UV Absorbent UV - 1164
Ji Jinling; Sun Lijiao; Huang Shanshan; Zhao Hui; Shi Chengyang; Wang Yunliang ∗;
(College of Pharmacy, Jiamusi University, Heilongjiang Jiamusi, 154007)
摘要:
对紫外吸收剂 UV - 1164 的合成工艺进行优化,以三聚氯氰为原料,一锅法合成关键中间体 2-(2,4-二羟基苯基)-4,6-二(2,4-二甲基苯基)-1,3,5-均三嗪(TM Ⅱ),再与溴辛烷反应合成紫外吸收剂 UV - 1164。 选取反应物物质的量比 n溴辛烷∶nTM Ⅱ、反应时间、反应温度 3 个因素,利用正交实验对合成进行优化,得到最佳合成条件:反应物物质的量比 n溴辛烷∶nTM Ⅱ 为 1∶1.2、反应时间为 2 h、反应温度为 70 ℃。 对优化后的工艺进行放大实验,产率稳定, 具有工业化应用潜质。
关键词：紫外吸收剂 UV - 1164；傅克烷基化反应；工艺优化；工艺放大；
Abstract：
The synthesis process of UV absorber UV - 1164 was optimized. The key intermediate 2 - (2,4 - dihydroxyphenyl) - 4,6 - bis(2,4 - dimethylphenyl) - 1,3,5 - triazine (TM Ⅱ) was synthesized by one-pot method with melamine as raw material. The UV absorber UV - 1164 was then synthesized by reaction with bromooctane. The molar ratio of reactant nbromooctane ∶ nTM Ⅱ, reaction time and reaction temperature were selected to optimize the synthesis by orthogonal test, and the optimum synthesis conditions were obtained: molar ratio of reactant nbromooctane ∶ nTM Ⅱ was 1∶ 1. 2, reaction time was 2 h, and reaction temperature was 70 ℃ . The results showed that the optimized process had stable yield and potential for industrial application.
Keywords：UV absorber UV - 1164; Fouke alkylation reaction; process optimization; scale-up;