N, N-二甲基三甲基硅胺的合成及表征
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TQ264.1

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江苏省绿色催化材料与技术重点实验室资助项目(BM2012110)


Synthesis and Characterization of N, N-dimethyltrimethylsilylamine
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    摘要:

    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)。研究了溶剂比、反应温度、催化剂用量、TMCS加料速度及反应时间对产物产率的影响,并对目标化合物进行了FTIR、1H NMR、GC表征。结果表明,当n(TMCS):n(TMB)=1:2,反应温度为30 ℃,催化剂用量为0.3 mL,TMCS滴加时间为15 min,反应时间为60 min时,DMATMS的收率为90.77%,纯度为97.31%。

    Abstract:

    The N, N-dimethyltrimethylsilylamine (DMATMS) was synthesized by reacting trimethylchlorosilane (TMCS) with dimethylamine catalyzed by timethylmethoxysilane in the solvent 1, 2, 4-trimethylbenzene(TMB). Effects of molar ratio of TMCS to TMB,reaction temperature, amount of catalyst, reaction time on the yield of DMATMS were investigated, and the target compound was characterized by means of FTIR, 1H NMR and GC. The results indicated 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 is 0.3 mL, feeding time of TMCS is 20 min, and reaction time was 60 min. After purification, the purity of DMATMS reaches 97.31%.

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马江权. N, N-二甲基三甲基硅胺的合成及表征[J].精细化工,2014,31(6):

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  • 收稿日期:2014-03-10
  • 最后修改日期:2014-04-03
  • 录用日期:2014-04-15
  • 在线发布日期: 2014-05-04
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