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首页> 外文期刊>Tetrahedron, Asymmetry: The International Journal for Repid Publication on all Aspects of Asymmetry in Orgainc, Inorganic, Organometallic, Physical and Bio-Organic Chemistry >Resolution of N-methylamphetamine enantiomers with tartaric acid derivatives by supercritical fluid extraction
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Resolution of N-methylamphetamine enantiomers with tartaric acid derivatives by supercritical fluid extraction

机译：超临界流体萃取分离酒石酸衍生物与N-甲基苯丙胺对映体

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摘要

The resolution of N-methylamphetamine (MA) was carried out With the resolution agents O,O'-dibenzoyl-(2R,3R)-tartaric acid monohydrate (DBTA) and O,O'-di-p-toluoyl-(2R,3R)-tartaric acid (DPTTA). After partial diastereomeric salt formation, the unreacted enantiomers ware extracted by supercritical fluid extraction (SEE). The effects of resolution agent molar ratio to the racemic Mixture (mr), extraction pressure (P) and temperature (T) on the resolution efficiency were studied. The best chiral separation was obtained at a quarter of an equivalent resolution agent molar ratio for both resolution agents. Extraction conditions [pressure (100-200 bar), temperature (33-63degreesC)] did not influence the resolution efficiency, which makes the enantiomer separation robust. In one extraction step, both enantiomers can be produced with high enantiomeric excess (ee) and remarkable yield (Y). Using DBTA as a resolution agent ee(E) = 83%, Y-E = 45% for the extract and ee(R) = 82%, Y-R = 42% for the raffinate were obtained. (C) 2004 Elsevier Ltd. All rights reserved.
机译：N-甲基苯丙胺（MA）的拆分是通过拆分剂O，O'-二苯甲酰基-（2R，3R）-酒石酸一水合物（DBTA）和O，O'-二-对甲苯甲酰基-（2R， 3R）-酒石酸（DPTTA）。在部分非对映异构体盐形成后，通过超临界流体萃取（SEE）萃取未反应的对映异构体。研究了拆分剂对消旋混合物的摩尔比（mr），萃取压力（P）和温度（T）对拆分效率的影响。两种拆分剂在等效拆分剂摩尔比的四分之一时可获得最佳的手性分离。萃取条件[压力（100-200 bar），温度（33-63℃）]不影响拆分效率，这使对映异构体的分离更加可靠。在一个萃取步骤中，两种对映体都可以高对映体过量（ee）和显着收率（Y）的方式生产。使用DBTA作为拆分剂，提取物的ee（E）= 83％，Y-E = 45％，萃余液的ee（R）= 82％，Y-R = 42％。 （C）2004 Elsevier Ltd.保留所有权利。

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