四氢糠酸的拆分工艺改进

利用非对映异构体盐在溶剂中溶解度的不同，以(1S,2R)-1-氨基-2-茚醇(1)为手性拆分剂，拆分四氢糠酸［(RS)-THFA, (RS)-2］获得高光学纯的(S)-2，其结构经¹H NMR, ¹³C NMR和HPLC确证。探究了不同溶剂量和投料比对拆分效果的影响。结果表明较佳拆分条件为：以4-甲基-2-戊酮(3)作溶剂，n［(RS)-2］: n(1)=2.2 : 1，一次拆分得91.7% ee (S)-2;再以n［91.7% ee (S)-2］: n(1)=6 : 5进行二次拆分得99.0% ee (S)-2。拆分剂的回收率提高至92.0%，同时对拆分母液中的非目标对映体成功地进行消旋化，回收率为89.0%，实现了四氢糠酸的循环拆分。

Process Improvement on Resolution of Tetrahydrofuran-2-carboxylic Acid

(S)-tetrahydrofuran-2-carboxylic acid ( S )-2 ] with high optical purity was resolved ac-cording the different dissolution of the diastereomeric salt , from rac-tetrahydrofuran-2-carboxylic acid (RS)-THFA, (RS)-2] using (1S,2R)-1-aminoindan-2-ol(1) as the resolving agent.The influ-ences of amount of solvent , the percentage of THFA and the resolving agent to the resolution were stud-ied.The optimum resolution conditions were as follows:using 4-methylpentan-2-one(3) as solvent, n (RS)-2] :n(1)=2.2 :1, the first resolution turns out 91.7％ ee (S)-2.99.0％ ee (S)-2 was prepared by second resolution with n91.7％ee ( S)-2] :n(1) of 6:5.The recycling resolution was realized with the recovery of 92.0％of the resolving agent as well as 89.0％of THFA which was race-mized by the non target enantiomeric isomer from mother liquor .