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文章编号: 1672-6987(2020)01-0018-04; DOI: 10.16351/j.1672-6987.2020.01.002
王少娟, 刘俊宏, 吴鸿志, 杨晶巍, 唐林生*
(青岛科技大学 化工学院,山东 青岛 266042)
摘要: 以1-甲氧基-4-羟基-2,2,6,6-四甲基哌啶醇(简称哌啶醇)和三氯化磷为原料,合成亚磷酸三(1-甲氧基-2,2,6,6-四甲基哌啶)酯,并通过IR、1H NMR、13C NMR和31P NMR对产品结构进行了表征。结果表明,其较佳的合成工艺条件:三乙胺为缚酸剂,氯仿为溶剂,n(PCl3)∶n(哌啶醇)∶n(三乙胺)=1∶300∶450,在30 ℃反应8 h。在此条件下,目标产物的收率为8336%,磷摩尔分数大于99%。
关键词: 亚磷酸三(1-甲氧基-2,2,6,6-四甲基哌啶基)酯; 1-甲氧基-4-羟基-2,2,6,6-四甲基哌啶醇; 三氯化磷
中图分类号: TQ 314.24文献标志码: A
引用格式: 王少娟, 刘俊宏, 吴鸿志, 等. 亚磷酸三(1-甲氧基-2,2,6,6-四甲基哌啶基)酯的合成\[J\]. 青岛科技大学学报(自然科学版), 2020, 41(1): 18-21.
WANG Shaojuan, LIU Junhong, WU Hongzhi, et al. Synthesis of tris(1-methoxy-2,2,6,6-tetramethylpiperidin-4-yl)phosphite\[J\]. Journal of Qingdao University of Science and Technology(Natural Science Edition), 2020, 41(1): 18-21.
Synthesis of Tris(1-methoxy-2,2,6,6-tetramethylpiperidin-4-yl)Phosphite
WANG Shaojuan, LIU Junhong, WU Hongzhi, YANG Jingwei, TANG Linsheng
(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042,China)
Abstract: Tris(1-methoxy-2,2,6,6-tetramethyl piperidine-4-yl)phosphite was synthesized by using 1-methoxy-2,2,6,6-tetramethyl piperidine-4-ol(piperidinol) and phosphorus trichloride as raw materials, and its structure was characterized by IR, 1H NMR, 13C NMR and 31P NMR. The results revealed that its optimal conditions were as follows: triethylamine as acid-binding agent, chloroform as solvent, n(PCl3)∶n(piperidinol)∶n(triethylamine)=1∶300∶450, the reaction 8 h at 30 ℃. Under the above conditions, the yield of the target products was 8336%, and the molar content based all phosphorus compound was more than 99%.
Key words: tris(1-methoxy-2,2,6,6-tetramethyl piperidine-4-yl)phosphite; 1-methoxy-2,2,6,6-tetramethyl piperidine-4-ol; phosphorus trichloride
收稿日期: 2019-01-04
基金项目: 山东省教育厅科技计划项目(J16LC21);山东省自然科学基金项目(ZR2015BL025).
作者简介: 王少娟(1991—),女,硕士研究生.*通信联系人.