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PROCESS FOR PREPARING (+)2-(4-CHLOROPHENYL)-3-METHYL BUTANOIC ACID

机译:制备(+)2-(4-氯苯基)-3-甲基布丁酸的方法

摘要

The present invention relates to an environmentally benign process for preparation of (+)2-(4-chlorophenyl)-3-methyl butanoic acid (+ CPA) from 2s6 racemic acid, using optically active arylamines like (-) PEA in hydrophilic/hydrophobic organic solvents like butanol, propanol etc. as aqueous mixtures, separating the desired (+) CPA salt, mother liquor by filtration and refining the (+) CPA salt in the same solvent system as used for resolution, recovering the desired acid in high optical purity by extracting with aqueous mineral acid. The mother liquor is concentrated under vacuum and extracted with aqueous mineral acid to obtain undesired (-) CPA which was recovered and recycled after racemization. The aqueous mineral acid layer thus obtained is mixed with corresponding aqueous mineral acid layer obtained from (+) CPA recovery and extracted with aqueous caustic lie solution to recover the optically active amine used for resolution. Thus the method described effectively provides a process for recovery and recycle of the undesired (-) CPA, optically active amine, besides obtaining the desired (+) CPA in high optical purity.
机译:本发明涉及一种环境友好的方法,该方法从2s6外消旋酸制备(+)2-(4-氯苯基)-3-甲基丁酸(+ CPA),使用光学活性芳胺如(-)PEA在亲水/疏水中有机溶剂(例如丁醇,丙醇等)作为水性混合物,通过过滤分离所需的(+)CPA盐,母液,并在与用于分离的溶剂系统相同的溶剂系统中精制(+)CPA盐,从而在高光学条件下回收所需的酸通过用无机酸水溶液萃取来纯化纯度。将母液在真空下浓缩并用无机酸水溶液萃取以获得不希望的(-)CPA,将其回收并在外消旋后再循环。将由此获得的无机酸水溶液层与从(+)CPA回收中获得的相应的无机酸水溶液层混合,并用苛性碱水溶液萃取以回收用于拆分的光学活性胺。因此,除了获得高光学纯度的所需(+)CPA之外,所描述的方法有效地提供了用于回收和再循环不希望的(-)CPA,光学活性胺的方法。

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