无溶剂合成Me3SiOMeRSiMe3〔R=O(CH2)2N(CH3)2〕的研究

Solvent free synthesis of intermediate for

摘要:

利用无溶剂加热方法，以N，N－二甲基乙醇胺(DMEA)和七甲基三硅氧烷（MDHM）为原料，合成Me3SiOMeRSiMe3〔R=O(CH2)2N(CH3)2〕。讨论了反应中反应时间，反应温度，反应物摩尔比，催化剂浓度等因素对反应转化率的影响。采用正交实验，对以无溶剂加热法合成MDHM型三硅氧烷叔胺的工艺进行优化，并利用减压蒸馏分离提纯和气相色谱技术确定纯后产物纯度，并且经过质谱分析和核磁共振鉴定产物的结构。

Abstract:

MeSiOMeRSiMe3〔R=O(CH2)2N(CH3)2〕was synthesized in solvent-free with dimethylethanolamine (DMEA ) and Heptamethyltrisiloxane（MDHM）as raw materials. Reaction time, reaction temperature, reactant molar ratio，catalyst concentration on the reaction conversion rate influence was discussed. Through orthogonal experiment, the solvent-free synthesis technique of MeSiOMeRSiMe3〔R=O(CH2)2N(CH3)2〕 was optimized. The purification of the target product by reduced pressure distillation and the The purity of the purified product measure by gas phase chromatography. The structure of the product was characterized by mass spectrum and 1H NMR.