摘要
以含氯烃基的硅氧烷同邻烯丙基苯酚进行威廉逊反应,制得了几种含烯丙基的硅氧烷。在浓硫酸催化下,1,3-双氯甲基-四甲基二硅氧烷(Ⅰ)同八甲基环四硅氧烷反应得到α,ω-双氯甲基-二甲基硅氧烷低聚物(Ⅱ);将Ⅰ或Ⅱ同过量的邻烯丙基苯酚在乙醇中回流反应8 h,分别得到1,3-双(邻烯丙基苯氧甲基)-1,1,3,3-四甲基二硅氧烷和α,ω-双(邻烯丙基苯氧甲基)-二甲基硅氧烷低聚物;室温下,γ-氯丙基甲基二甲氧基硅烷(Ⅲ)水解得到γ-氯丙基甲基硅氧烷低聚物(Ⅳ),Ⅲ同氯甲基二甲基氯硅烷共水解得到氯甲基封端的γ-氯丙基甲基硅氧烷低聚物(Ⅴ);在氢氧化钾作用下,用四丁基溴化铵为催化剂,将Ⅳ或Ⅴ同邻烯丙基苯酚在二甲基甲酰胺中回流反应16 h,分别得到γ-(邻烯丙基苯氧基)丙基甲基硅氧烷低聚物和α,ω-双(邻烯丙基苯氧甲基)-γ-(邻烯丙基苯氧基)丙基甲基硅氧烷低聚物。用1H NMR和IR等方法对产物的结构进行了表征。
Several allyl-containing siloxanes were synthesized from chloroalkyl siloxanes and o-allyl phenol by Williamson reaction.With the concentrated sulfuric acid as the catalyst,1,3-bis（chloromethyl）-1,1,3,3-tetramethyl-disiloxane（I） reacted with octamethylcyclotetrasiloxane to obtain α,ω-bis（chloromethyl） dimethyl siloxane oligomer（II）.1,3-bis（o-allyl phenoxymethyl）-1,1,3,3-tetramethy-disiloxane or α,ω-bis（o-allyl phenoxymethyl）-capped dimethyl siloxane oligomer was synthesized from I or II,and excess amount of o-allyl phenol by refluxing for 8 hours in ethanol.At room temperature,γ-chloropropyl methyl dimethoxysilane（III） was hydrolyzed to obtain γ-chloropropyl methyl siloxane oligomer（IV）;meanwhile,III was cohydrolyzed with chloromethyl dimethyl chlorosilane to obtain γ-chloropropyl methyl siloxane oligomer capped with bis-chloromethyl group（V）.In the presence of potassium hydroxide and with tetrabutylammonium bromide as the catalyst,γ-（o-allyl phenoxy）-propyl methyl siloxane oligomer or α,ω-bis（o-allyl phenoxymethyl）-capped γ-（o-allyl phenoxy）-propyl methyl siloxane oligomer was prepared respectively from IV or V,and o-allyl phenol by refluxing for 16 hours in N,N-dimethyl formamide.1H NMR and IR were applied to characterize the structure of the products.
出处
《有机硅材料》
CAS
2011年第4期219-224,共6页
Silicone Material
