摘要
为了探寻1-萘基三甲氧基硅烷新的合成工艺,以四甲氧基硅烷和1-溴代萘为原料,采用钠缩法在无外加溶剂的条件下得到1-萘基三甲氧基硅烷。采用平行实验优选法优化了1-萘基三甲氧基硅烷的合成工艺,发现实验的最佳反应条件为8.28 g金属钠(0.36 mol),150 mL四甲氧基硅烷,加热温度设定为90~100℃,逐滴加入25 mL 1-溴代萘(0.18 mol),在6 h内滴加完毕。调节1-溴代萘的滴加速度并控制反应温度在70℃,滴加结束后将反应釜温设定为100~110℃,在此条件下继续搅拌3 h,粗产物产率可达到74%。该合成工艺产率较高,过程简单,操作安全。
Tetramethoxysilane and 1-bromonaphthalene were used to obtain 1-naphthyltrimethoxysilane via sodium condensation without external solvent,to enquire a new synthesis process of 1-naphthyltrimethoxysilane.The synthesis of 1-naphthyltrimethoxysilane was optimized by the preferred method of parallel experiments.The optimal reaction conditions for the experiment were found to be 8.28 g of sodium(0.36 mol),150 mL of tetramethoxysilane,with the heating temperature at 90~100℃,and 25 mL of 1-bromonaphthalene(0.18 mol)was added dropwise within 6 h.The drop acceleration of 1-bromonaphthalene was adjusted,the reaction temperature was controlled at 70℃,and the reaction tank temperature was set at 100~110℃after drop addition.The reaction was stirred for another 3 h under this condition and the crude product yield could be up to 74%.The synthetic process has high yield,simple process and safe operation.
作者
万水
李强
彭游
焦艳晓
WAN Shui;LI Qiang;PENG You;JIAO Yan-xiao(College of Chemistry and Chemical Engineering,Jiujiang University,Jiangxi Jiujiang 332005;Jiujiang Yuren New Materials Co.,Ltd.,Jiangxi Jiujiang 332105,China)
出处
《广州化工》
CAS
2022年第22期65-67,共3页
GuangZhou Chemical Industry
基金
九江市留学人员成果转化支持计划(20200410)
九江市重点研发计划(S2021ZDYFG031)。
关键词
武兹反应
萘基烷氧基硅烷
钠缩法
Wutz reaction
naphthalyl alkyoxysilane
sodium condensation
