直链淀粉-三(苯基氨基甲酸酯)手性固定相的制备及对外消旋硫代缩水甘油醚的直接拆分

Direct Enantiomeric Resolution of Thio-glycidyl Ether Using Amylose-Tris(phenylcarbamate) Chiral Stationary by High Performance Liquid Chromatography

在参照文献基础上，合成并制备了直链淀粉－三（苯基氨基甲酸酯）手性固定相，利用高效液相色谱首次直接拆分了４种外消旋硫代缩水甘油醚，并考察了流动相中异丙醇含量对拆分的影响。

We have synthesized amylose- tris (phenylcarbamate), and coated it on the silica gel as chiral stationary phase. This stationary phase offered a practically useful chiral column with a high enantiomerseparability. Amylose was allowed to react with an excess of phenylisocyanate in pyridine for 48 h. The obtained carbamates was dissolved and adsorbed on silica gel which has been treated with 3- aminopropyltriethoxysilane. The weight ratio of the carbamate to the silica gel was 0 .45/2. 55. The four thio-glycidyl ether were resoluted on amylose tris(phenylcarbamate) chiral stational phase. Separation was carried out with a hexane/2-propanol mixture at a flow rate of 1 .0 mL/min at temperature temperature. The effects of 2- propanol concentration on the retention and resolution were investigated.