Preparative enantioseparation of propafenone by counter-current chromatography using di-n-butyl L-tartrate combined with boric acid as the chiral selector

Preparative enantioseparation of propafenone by counter-current chromatography using di-n-butyl L-tartrate combined with boric acid as the chiral selector
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L-酒石酸二正丁酯与硼酸作为手性选择剂逆流色谱法制备普罗帕酮对映体分离

DOI:
10.1002/jssc.201300614
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发表时间:
2013-09-01
影响因子:
3.1
通讯作者:
Yan, Jizhong
Yan, Jizhong
中科院分区:
工程技术3区
文献类型:
--
作者:
Tong, Shengqiang;Shen, Mangmang;Yan, Jizhong

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This paper extends the research of the utilization of borate coordination complexes in chiral separation by counter-current chromatography (CCC). Racemic propafenone was successfully enantioseparated by CCC with di-n-butyl L-tartrate combined with boric acid as the chiral selector. The two-phase solvent system was composed of chloroform/0.05 mol/L acetate buffer pH 3.4 containing 0.10 mol/L boric acid (1:1, v/v), in which 0.10 mol/L di-n-butyl L-tartrate was added in the organic phase. The influence of factors in the enantioseparation of propafenone were investigated and optimized. A total of 92 mg of racemic propafenone was completely enantioseparated using high-speed CCC in a single run, yielding 40-42 mg of (R)- and (S)-propafenone enantiomers with an HPLC purity over 90-95%. The recovery for propafenone enantiomers from fractions of CCC was in the range of 85-90%.