格氏试剂法合成二环戊基二甲氧基硅烷的研究

Synthesis of Dicyclopentyl Dimethoxy Silane by Gringard Reaction

研究了格氏试剂法合成二环戊基二甲氧基硅烷(D Donor)的工艺。用氯代环戊烷与镁粉、四甲氧基硅烷在溶剂甲苯中同时完成格氏化反应和取代反应,经分离、精馏得二环戊基二甲氧基硅烷。四甲氧基硅烷74mL(0 5mol)、镁粉30g(1 25mol)、THF100mL、氯代环戊烷10mL,在氮气保护下回流,滴加105mL氯代环戊烷和500mL甲苯的混合液,回流5h。过滤、精馏得二环戊基二甲氧基硅烷89 3g,纯度99%,收率78 2%。

The synthesis of dicyclopentyl dimethoxy silane was studiedThe gringard and replacement reaction between tetramethyl orthosilicate and chlorocyclopentane with magnesium were took place in the solventsDicyclopentyl dimethoxy silane was obtained by separation and rectification74 mL(05 mol) Tetramethyl orthosilicate and 30 g(125 mol) magnesium,100 mL THF and 10 mL chlorocyclopentane were refluxed in nitrogen atmosphere.105 mL Chlorocyclopentane and 500 mL methylbenzene were added dropwise to the systemAfter 5 h,893 g dicyclopentyl dimethoxy silane(in 782% yield and 99% purity) was obtained by separation and rectification