机构地区: 广州大学化学化工学院
出 处: 《精细化工》 2007年第11期1091-1094,共4页
摘 要: 以(S)-(+)-樟脑磺酰氯作柱前手性衍生化试剂,与外消旋1,1′-联-2-萘酚反应,形成非对映异构体联二萘酚樟脑磺酸酯,再用反相高效液相色谱进行分离。结果表明,采用Zorbax XDB-C8和HypersilODS(C18)柱,流动相V(甲醇)∶V(水)分别为75∶25和85∶15,流速均为1mL/min时,分离度分别为1.86和1.74,有效地分离了两个非对映异构体。进一步水解得到光学纯(R)-1,1′-联-2-萘酚和(S)-1,1′-联-2-萘酚,ee值均达99%以上。 As the precolumn derivating agent, (S)-( + )-camphorsulfonyl chloride reacted with the raccmic ( ± )-1,1 '-bi-2-naphthol, producing two diastereomers of bis ((S)-camphorsulfonates). Then the diastereomers were separated by reverse-phase high performance liquid chromatography. The result showed that the Zorbax XDB -C8 or Hypersil ODS( C18 ) column and V( methanol ) : V( water ) = 75:25 or 85:15 as eluent at a flowrate of 1 mL/min are suitable for the separation. Hydrolysis of the eluent gave optically pure (R)-and (S)-1,1 '-bi-2-naphthol with ee 〉 99%.