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SEPARATION OF N-METHYLAMPHETAMINE ENANTIOMERS BY SUPERCRITICAL FLUID EXTRACTION

机译:超临界流体萃取分离N-甲基苯丙胺对映体

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Separation of N-methylamphetamine enantiomers was carried out using O,O'-di-p-toluoyl-(2R,3R)-tartaric acid as a resolution agent in less than equivalent molar ratio. After the partial diastereomeric salt formation, the unreacted enantiomers were extracted with supercritical carbon dioxide. The effects of the resolution agent molar ratio, extraction pressure and temperature on the resolution efficiency were studied. The maximal chiral separation was obtained at quarter of an equivalent resolution agent molar ratio. Changing of the extraction pressure (100-200 bar) and temperature (33-63℃) has no significant effect on the resolution efficiency, which makes the separation robust. In one extraction step both enantiomers can be produced with high optical purity and remarkable yield (OP_E = 68%, Y_E = 45 % for the extract and OP_R = 70 %, Y_R = 40 % for the raffinate).
机译:使用小于当量摩尔比的O,O′-二对甲苯甲酰基-(2R,3R)-酒石酸作为拆分剂进行N-甲基苯丙胺对映体的分离。在部分非对映异构体盐形成后,用超临界二氧化碳萃取未反应的对映异构体。研究了拆分剂摩尔比,萃取压力和温度对拆分效率的影响。在等效拆分剂摩尔比的四分之一处获得最大的手性分离。萃取压力(100-200 bar)和温度(33-63℃)的变化对分离效率没有显着影响,这使分离更加牢固。在一个萃取步骤中,两种对映异构体均可以高光学纯度和显着产率生产(萃取液的OP_E = 68%,Y_E = 45%,萃余液的OP_R = 70%,Y_R = 40%)。

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