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.