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双(N,N-二乙基)胺基甲基三氟丙基硅烷合成研究
引用本文:伍川,胡从达,董红,杨雄发,蒋剑雄.双(N,N-二乙基)胺基甲基三氟丙基硅烷合成研究[J].杭州师范学院学报(自然科学版),2009,8(4):282-285.
作者姓名:伍川  胡从达  董红  杨雄发  蒋剑雄
作者单位:杭州师范大学有机硅化学及材料技术教育部重点实验室,浙江杭州,310012
基金项目:教育部重点科研项目,浙江省自然科学基金项目 
摘    要:以甲基三氟丙基二氯硅烷和二乙胺为原料,低温反应合成了含氟硅聚酰亚胺材料的重要中间体双(N,N-二乙基)胺基甲基三氟丙基硅烷,利用红外光谱、核磁共振及质谱等手段对产物结构进行了表征和确认.利用正交实验考察了反应温度、反应时间、原料摩尔比以及溶剂组成等因素对目标产物收率的影响,基于方差分析确定出最佳反应条件为:反应时间6h,反应温度-10℃,二乙胺与甲基三氟丙基二氯硅烷的比例为6:1,溶剂为乙醚与二氯甲烷的等体积混合物.正交实验结果经重复实验得到验证.

关 键 词:双(N  N-二乙基)胺基甲基三氟丙基硅烷  甲基三氟丙基二氯硅烷  正交实验  方差分析

Synthesis of Bis(N, N-diethylamino)methyltrifluoropropylsilane
WU Chuan,HU Cong-da,DONG Hong,YANG Xiong-fa,JIANG Jian-xiong.Synthesis of Bis(N, N-diethylamino)methyltrifluoropropylsilane[J].Journal of Hangzhou Teachers College(Natural Science),2009,8(4):282-285.
Authors:WU Chuan  HU Cong-da  DONG Hong  YANG Xiong-fa  JIANG Jian-xiong
Institution:(Key Laboratory of Organosilicon Chemistry and Material Technology of Ministry of Education, Hangzhou Normal University Hangzhou 310012, China)
Abstract:Bis(N, N-diethylamino) methyltrifluoropropylsilane, one of the important intermediates of functional polyimides, is synthesized from diethylamine and methyltrifluoropropyldichlorosilane under low temperature and characterized by GC-MS, FT-IR, 1H NMR and ^13C NMR. An orthogonal experimental design is conducted and the influence of each factors, such as temperature, reaction time, solvents and the feeding ratio, on the yield of the objective product have been investigated. The optimal experimental condition is determined by means of variance analysis method with the following result, that is the reaction time is 6 h, reaction temperature is --10 ℃, the feeding ratio between diethylamine and methyltrifluoropropyldichlorosilane is 6 : 1 and the solvent is the equivalent volume mixture of ether and dichloromethane. The above optimal results are further verified by duplicate tests.
Keywords:Bis(N  N-diethylamino)methyltrifluoropropylsilane  methyltrifluoropropyldichlorosilane  orthogonal design method  variance analysis
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