1,3-双(3-氨丙基)-1,1,3,3-四甲基二硅氧烷的合成

Synthesis of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane

以二甲基一氯硅烷和γ-氯丙烯为原料,经硅氢加成得到γ-氯丙基二甲基氯硅烷,加成产物提纯后经水解缩合得到1,3-双(γ-氯丙基)四甲基二硅氧烷(简称氯丙基双封头),氯丙基双封头和液氨进行氨化反应后得到1,3-双(3-氨丙基)-1,1,3,3-四甲基二硅氧烷。对第一步硅氢加成反应的催化剂和反应条件进行优化,确定了最优合成工艺,使用2,2,6,6-四甲基-4-哌啶酮配合氯铂酸作催化剂,收率可达87.3%;第二步水解缩合反应收率为97.5%;第三步氨化反应考察了影响收率的影响因素,确定了最佳反应条件,收率为78.6%,经三步反应总收率为66.9%。

Using dimethyl monochlorosilane and γ-chloropropylene as raw materials,γ-chloropropyl dimethylchlorosilane was obtained by hydrosilylation.The addition product was purified and then hydrolyzed and condensed to obtain 1,3-bis(γ-chloropropyl)tetramethyldisiloxane(abbreviated as Chloropropyl double capping agent).1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane was obtained after amination reaction of chloropropyl double head and liquid ammonia.The catalyst and reaction conditions of the first hydrosilylation reaction were optimized,and the best synthesis process was determined.Using 2,2,6,6-tetramethyl-4-piperidone and chloroplatinic acid as catalysts,the yield was up to 87.3%;the yield of the second step of hydrolysis and condensation reaction was 97.5%;the factors affecting of the yield were investigated and the best reaction conditions were determined through the third step of amination reaction,the yield was 78.6%,the total yield after the three-step reaction was 66.9%.