乙氧丙嗪对映体的分离、溶液构象和绝对构型。

Enantiomer Pub Date : 2002-03-01 DOI:10.1080/10242430212188
G. Šinko, P. Novak, Dinko Žiher, V. Vinković, V. Sunjic, V. Simeon-Rudolf
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引用次数: 3

摘要

采用非对映体二苯甲酰酒石酸盐分步结晶法制备了乙氧丙嗪对映体盐酸(10-(2-二乙基氨基丙基)吩噻嗪),并在Chiralcel OJ柱上采用高效液相色谱法测定了其光学纯度(对映体过量,ee)。以正己烷/丁醇/三乙胺(100:3:0.5)为溶剂,对外消旋乙丙嗪进行了很好的对映分离(α = 1.68)。(-)-对映体纯度为99.1%,(+)-对映体纯度为97.9%。结合两种对映体的NMR和CD光谱数据,以及先前报道的外消旋乙氧丙嗪的x射线结构分析,揭示了溶液中三环体系的倾斜构象,(-)-对映体的立体中心为(S)构型,(+)-对映体的立体中心为(R)构型。
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Separation, conformation in solution and absolute configuration of ethopropazine enantiomers.
Enantiomers of ethopropazine x HCl (10-(2-diethylaminopropyl)phenothiazine hydrochloride) were prepared by fractional crystallization of diastereomeric dibenzoyltartaric acid salts, and their optical purity (enantiomeric excess, ee) determined by HPLC on Chiralcel OJ column. With a solvent mixture n-hexane/t-butanol/triethylamine (100:3:0.5) as eluent a very good enantioseparation (alpha = 1.68) for racemic ethopropazine was obtained. Enantiomeric purity for (-)-enantiomer was 99.1% and for (+)-enantiomer 97.9%. Combined data from NMR and CD spectra of both enantiomers, along with previously reported X-ray structure analyses of racemic ethopropazine, revealed skewed conformation of tricyclic system in solution, and (S)-configuration on the stereogenic center for (-)-enantiomer, and (R)-configuration for (+)-enantiomer.
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