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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 of racemic 1,1’-bi-2-naphthol [(±) -BINOL] was studied. Using cheap chiral dehydroabietylamine as the resolving agent, the effects of reaction time, amount of resolving agent, solvent ratio and (±) -BINOL concentration on (S) -BINOL and (R) - Impact of BINOL Yield. In the reaction time 1 h, n (dehydroabietylamine): n [(±) -BINOL] = 1: 1 and V (ethanol) 0.3 mol / L, the yields of (S) -BINOL and (R) -BINOL were 72.7% and 53.1%, respectively, and their ee values were all above 99%. The recoveries of the resolving agents were 90.5% . The novelty of this research work has been confirmed by Science and Technology Report No. 2009-234 issued by China National Chemical Information Center on September 18, 2009.