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1环己氧基4羟基2,2,6,6四甲基哌啶醇的合成

作者:时间:2018-07-10点击数:

PDF全文下载:  201804003.pdf

 

文章编号: 16726987201804002305 DOI 10.16351/j.16726987.2018.04.003

 

杨晶巍, 吴鸿志, 侯小敏, 赵静, 唐林生

(青岛科技大学 化工学院,山东 青岛 266042

 

摘要: 对以4羟基2,2,6,6四甲基哌啶氮氧自由基(ZJ701)和环己烷为原料,叔丁基过氧化氢为氧化剂,CuCl2·2H2O为催化剂,通过O烷基化反应合成1环己氧基4羟基2,2,6,6四甲基哌啶醇进行了研究。结果表明,较佳反应条件为:n(ZJ701)n(TBHP)n(CuCl2)n(环己烷)n(乙醇)=1960251335,反应时间为9 h,反应温度约65 ℃,较理想的提纯工艺为硼氢化物还原减压蒸馏重结晶。在以上条件下,目标产物的含量为9849%,分离产率为520%。该工艺反应条件温和,产品含量及收率较高。

关键词: 1环己氧基4羟基2,2,6,6四甲基哌啶醇; 4羟基2,2,6,6四甲基哌啶氮氧自由基; 环己烷; O烷基化反应

中图分类号: O 626.3文献标志码: A

引用格式: 杨晶巍, 吴鸿志, 侯小敏, . 1环己氧基4羟基2,2,6,6四甲基哌啶醇的合成\[J\]. 青岛科技大学学报(自然科学版), 2018 394): 2327.

YANG Jingwei, WU Hongzhi, HOU Xiaomin, et al. Synthesis of 1cyclohexyloxy2,2,6,6tetramethylpiperidine4ol\[J\]. Journal of Qingdao University of Science and TechnologyNatural Science Edition), 2018, 39(4) 2327.

 

Synthesis of 1Cyclohexyloxy2,2,6,6tetramethylpiperidine4ol

 

YANG Jingwei, WU Hongzhi, HOU Xiaomin, ZHAO Jing, TANG Linsheng

(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China)

 

Abstract: 1Cyclohexyloxy2,2,6,6tetramethylpiperidine4ol was synthesized by Oalkylation reaction by using 4hydroxy2,2,6,6tetramethylpiperidinooxy((ZJ701) and cyclohexane as raw materials, tertbutyl hydroperoxide (TBHP) as oxidant, CuCl2 as catalyst. The results revealed that its optimal conditions were as follows: n(ZJ701)n(TBHP)n(CuCl2)n(cyclohexane) n(ethanol) = 1960251335, the reaction time being 9h, and the reaction temperature being 65 , and optimal separation process was borohydride reduction vacuum distillationrecrystallation. Under the above conditions, the separated yield of the products was 520% and the purity was 9849%. The process has some advantages such as mild reaction condition, higher yield and purity.

Key words: 1cyclohexyloxy2,2,6,6tetramethylpiperidine4ol; 4hydroxy2,2,6,6tetramethylpiperidinooxy; cyclohexane; Oalkylation reaction

 

收稿日期:  20170516

基金项目: 山东省自然科学基金项目(ZR2015BL025);山东省教育厅科技计划项目(J16LC21.

作者简介: 杨晶巍(1976—),女,助理研究员.

 

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