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利用无溶剂加热方法,以N,N-二甲基乙醇胺(DMEA)和1,1,1,3,5,5,5-七甲基三硅氧烷(MDHM)为原料,合成了(Me3SiO)2Si(Me)(OC2H4)NMe2。考察了反应时间、反应温度、反应物摩尔比、催化剂浓度等因素对反应收率的影响。通过正交实验分析法得出最佳合成条件为:MDHM和DMEA的摩尔比为1.5∶1,反应时间为25min,反应温度为100℃,催化剂用量(占反应体系总质量的百分数,下同)为0.000 8%,在该条件下,最高收率为75.6%。利用减压蒸馏分离提纯和气相色谱技术确定提纯后产物纯度,并且经过质谱分析和核磁共振波谱鉴定产物的结构。
Using solvent-free heating method, N, N-dimethylethanolamine (DMEA) and 1,1,1,3,5,5,5-heptamethyl trisiloxane (MDHM) ) 2Si (Me) (OC2H4) NMe2. The effects of reaction time, reaction temperature, molar ratio of reactants and catalyst concentration on the reaction yield were investigated. Orthogonal experimental analysis obtained the best synthesis conditions: the molar ratio of MDHM to DMEA is 1.5: 1, the reaction time is 25min, the reaction temperature is 100 ℃, the amount of catalyst (as a percentage of the total mass of the reaction system, the same below) 0.000 8%. Under this condition, the highest yield was 75.6%. Purification by vacuum distillation and gas chromatography were used to determine the purity of the purified product, and the structure of the product was identified by mass spectrometry and nuclear magnetic resonance spectroscopy.