多糖聚合物手性固定相高效液相色谱法拆分二苯甲醇类手性化合物

目的：对6个氯取代的二苯甲醇类手性化合物建立HPLC分析方法。对拆分反应进行监测，并用于拆分产物光学纯度的分析测定。方法：在正相高效液相模式下，采用Chiralcel OD—H和Chiralcel OB-H两种纤维素类手性柱以及Chiralpak AD—H直链淀粉类手性柱，以正己烷-异丙醇或正己烷-异丙醇-三氟乙酸溶剂系统为流动相，流速：0．5ml·min^-1，检测波长：210nm。结果：采用上述方法，基线拆分了合成手性中枢性镇咳药左旋盐酸氯哌啶（-）cloperastine hydrochloride]的主要原料4-氯二苯甲醇等6个氯取代的二苯甲醇类手性化合物，建立了快速的手性高效液相色谱法。结论：本方法简便准确，可对手性合成反应进行监测和中间体质量控制;同时．对4-氯二苯甲醇和3-氟二苯甲醇的高效液相手性分析方法进行了对比研究。

HPLC Separation of Chlorobenzhyldrol Derivatives by Polysaccharide Derivatives Chiral Stationary Phases

Objective： To build up an HPLC method for chiral separation of chlorobenzhyldrol derivatives, to monitor the process of separation reaction and to determine the optical purity of the product. Method： Normal-phase high performance liquid chromatography with Chiralcel OD-H , Chiralcel OB-H and Chiralpak AD-H chiral columns were used. The detective wavelength was 210 nm, The mobile phase was recommended as Hexane-i-propanol or Hexane-i-propanol-TFA, with the flow rate was 0.5 ml· min^-1. Result： 4-Chlorobenzhyldrol, one of the major starting materials for synthesis of （-）-cloperastine hydrochloride, together with five chlorobenzhyl- drol chiral compounds was separated under the above conditions. Conclusion： With convenient and accurate, the methods for the chiral separation were established to monitor the process of the synthesis of D-4-chlorobenzhyldrol and to determine the optical purity of the product, side product and intermediates. In addition, the difference between 4-chlorobenzhyldrol and 3-chlombenzhyldrol on CSP was also discussed.