2,2,4-三甲基-2-硅杂吗啉的合成

Synthesis of 4-Methyl-2,2-dimethyl-2-silamorpholine

研究了氯甲基二甲基氯硅烷与β-氨甲基乙醇反应制备2,2,4-三甲基-2-硅杂吗啉的方法,考察了反应温度、反应物的配比优化和中和试剂的种类对合成产率的影响,确立了最佳的合成条件:反应物氯甲基二甲基氯硅烷与β-氨甲基乙醇的摩尔比为1∶1.05,甲苯为溶剂,三乙胺为中和试剂,其用量三乙胺与氯甲基二甲基氯硅烷的摩尔比为2.2∶1,醇解反应温度为65℃,收率可达75%,并采用波谱分析确证了目标物质的结构。

Chloromethyldimethylchlorosilane reacted with β-(methyl amino)ethanol to form 4-methyl-2,2-dimethyl-2-silamorpholine.The effect of reaction temperature,reagent flow and different neutralization agents and the solvent on the yield of 4-methyl-2,2-dimethyl-2-silamorpholine was studied.The experiment revealed that the reaction could be easily performed in toluene at 65 ℃,with n(Chloromethyldimethylchlorosilane)∶n[β-(methylamino)ethanol]=1∶1.05,n(triethylamine)∶n(Chloromethyldimethylchlorosilane)=2.2∶1,to give the yield of 75% for 4-methyl-2,2-dimethyl-2-silamorpholine.The structure was identified by Spectrum(H,IR)analysis.