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机构地区:[1]广西化工研究院,广西南宁530001 [2]广西师范学院,广西南宁530001
出 处:《精细化工》2010年第1期57-59,共3页Fine Chemicals
基 金:广西科学基金项目(0639016);广西培养新世纪学术和技术带头人专项资金资助项目(2004224)~~
摘 要:对外消旋1,1′-联-2-萘酚〔(±)-BINOL〕的拆分方法进行了研究。以廉价的手性脱氢枞胺为拆分剂,用正交实验法考察了反应时间、拆分剂用量、溶剂配比、(±)-BINOL浓度对(S)-BINOL和(R)-BINOL产率的影响。在反应时间1 h、n(脱氢枞胺)∶n〔(±)-BINOL〕=1∶1、V(乙醇)∶V(水)=4∶1、c〔(±)-BINOL〕=0.3 mol/L的最佳条件下,(S)-BINOL和(R)-BINOL的收率分别为72.7%和53.1%,它们的ee值均大于99%,拆分剂的回收率为90.5%。该文研究工作的新颖性已为中国化工信息中心2009年9月18日出具的第2009-234号《科技查新报告》所证实。The resolution process of racemic 1,1′-bi-2-naphthol((±)-BINOL) is studied in this article.The inexpensive dehydroabietylamine were taken as the split reagent.The effects of the reaction time,the quantity of split reagent,the composition of solvention and the concentration of reaction on the yield of(S)-BINOL and(R)-BINOL were also examined via the orthogonal experiment.Under the optimal conditions:reaction time 1 h,n(dehydroabietylamine)∶n((±)-BINOL)=1∶1,V(C2H5OH)∶V(H2O)=4∶1,c((±)-BINOL)=0.3 mol/L,the yield of(S)-BINOL and(R)-BINOL are 72.7% and 53.1% respectively.The ee value is more than 99% and the recovery of dehydroabietylamine was 90.5%.The novelty of this research work has been confirmed in the Science and Technology Novelty Search Report No.2009-234 by the China Chemical Industry Information Center on September 18,2009.
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