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机构地区:[1]台州职业技术学院生化学院生化研发中心,浙江台州318000
出 处:《应用化工》2013年第4期763-764,767,共3页Applied Chemical Industry
基 金:浙江省台州市科技计划项目资助(111KY01)
摘 要:以6,8-二氯辛酸乙酯为原料,水为溶剂和少量乙醇作为助溶剂,通过水解、环合和酸化3步合成硒辛酸,反应过程在均相中进行,且最终产品硒辛酸可直接从水相中析出,不需要用大量有机溶剂进行萃取。选取二硒化二钠滴加时间、二硒化二钠滴完后的反应温度和反应时间作为影响因素进行正交优化,得到最优反应条件为:滴加时间为2 h,反应温度为70℃,反应时间为3 h,反应总收率达到73%。The synthetic route of 6,8-diselenooctanoic acid was developed from ethyl 6,8-dichlorooctanoate via three steps, that is hydrolysis, selenylation and acidification, with water as a solvent and a small amount of ethanol as a co-solvent. The reaction process is carried out in a homogeneous phase, and the final product 6,8-diselenooctanoic acid can be directly precipitated from the aqueous phase, which was ever ex- tracted with a lot of organic solvent according to literature. Using dripping time of sodium diselenide, reaction temperature and time after dripping off sodium diselenide as the influencing factors to carry out the orthogonal experiment, and the best reaction conditions were as follows:the dripping time was 2 h, reaction temperature was 70 ℃ ,reaction time was 3 h and the total yield was 73%.
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