以十三氟辛醇和氯丙烯为原料、四丁基溴化铵为相转移催化剂,制得十三氟辛基烯丙基醚;再与甲基二氯硅烷进行硅氢加成反应,得到十三氟辛氧丙基甲基二氯硅烷。以核磁、红外及质谱对中间体和目标产物结构进行了表征,探索了十三氟辛基烯丙基醚、十三氟辛氧丙基甲基二氯硅烷的合成工艺。结果表明,合成十三氟辛基烯丙基醚的较佳工艺是:十三氟辛醇与烯丙基氯的量之比为1:1.2。于42℃反应24h:合成十三氟辛氧丙基甲基二氯硅烷的较佳工艺是:十三氟辛基烯丙基醚与甲基二氯硅烷的量之比为1:112.在Karstedt’s催化剂催化下反应3h。按照最优工艺合成十三氟辛氧丙基甲基二氯硅烷的总收率为65.7%。
Tridecafluorooctylally!ether~ was prepared by catalytic condensation, with tetrabutylammonium bromide as the phase transfer catalyst, tridecafluorooctanol and allyl chloride as the raw materials. Subse- quently, the tridecafluorooctylallylether was allowed to react with methyldichlorosilane to give the tridecafluo- rooctyloxapropylmethyl dichlorositane by hydrosilylation. The structures of the intermediates and target prod- ucts were characterized by ~H NMR, IR and MS. The synthetic reaction conditions were optimized, The opti- mal process of the synthesis of tridecafluorooctyl allyl ether was as follows : the molar ratio of tridecafluoroocta- nol to allyl chloride was 1 : 1.2, reacting at 42 ~C for 24 hours ; the optimal process of the synthesis of tridecaf- luorooctyloxapropylmethyldichlorosilane was using Karstedt's catalyst at tridecafluorooctyl allyl ether to dichlo- romethylsilane molar ratio of 1 : 1.2 for 3 hours. As a result, the total yield of tridecafluorooctyloxapropyl- methyldichlorosilane was up to 65.7%.