1,2-二(三甲基硅氧基)环已烯的合成

Synthesis of 1,2-Bis(trimethylsiloxy) Cyclohexene

生物素关键中间体1,2-二(三甲基硅氧基)环已烯的合成方法很多,采用1,2-环已二酮、双(三甲基硅)硫酸酯与活性金属在惰性溶剂中反应得到1,2-二(三甲基硅氧基)环已烯。而双(三甲基硅)硫酸酯可利用该反应中的副产物三甲基硅醇脱水得六甲基二硅氧烷,继续与浓硫酸反应制得。该工艺可实现硅保护基的循环利用,从根本上解决六甲基二硅氧烷废液的环保问题,工艺对环境友好。

The principal product 1,2-bis(trimethylsiloxy)cyclohexene as the key intermediate of biotin was synthesized by the reaction of 1,2-cyclohexanedione,bis-(trimethylsilyl)sulfate and active metal in inert solvent.The by-product of the reaction,trimethylsilanol,was dehydrated to get hexamethyldisiloxane,which was further reacted with concentrated sulfuric acid to get bis-(trimethylsilyl)sulfate,which was the raw material.The recycling of silicon protective base can be realized,with the environmental protection problem caused by waste liquid solved fundamentally by the process,which was environmentally friendly.