N,N-二甲基三甲基硅胺的合成及表征

Synthesis and Characterization of N,N-Dimethyltrimethylsilylamine

以三甲基氯硅烷(TMCS)、二甲胺为起始原料,偏三甲苯(TMB)为溶剂,经甲氧基三甲基硅烷催化合成N,N-二甲基三甲基硅胺(DMATMS)。考察了溶剂比、反应温度、催化剂用量、TMCS加料速度及反应时间对产物收率的影响,并对目标化合物进行了FTIR、1HNMR、GC表征。结果表明,当n(TMCS)∶n(TMB)=1∶2,反应温度30℃,催化剂用量0.3 mL,TMCS滴加时间15 min,反应时间60 min时,DMATMS收率90.77%,质量分数97.31%。

N, N-dimethyltrimethylsilylamine （ DMATMS ） was synthesized by reacting trimethylchlorosilane （TMCS） with dimethylamine catalyzed by trimethylmethoxysilane in the solvent 1, 2,4-trimethylbenzene （TMB）. Effects of molar ratio of TMCS to TMB, reaction temperature, amount of catalyst, feeding time of TMCS and reaction time on the yield of DMATMS were investigated, and the target compound was characterized by means of FTIR, 1HNMR and GC. The results indicate that the highest yield of DMATMS was 90.77% when the molar ratio of TMCS to TMB was 1：2 ,the reaction temperature was 30℃, amount of catalyst was 0. 3 mL, feeding time of TMCS was 15 min, and reaction time was 60 min. After purification, the purity of DMATMS reached 97.31%.