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New method for preparation of D-valine

机译:制备D-缬氨酸的新方法

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摘要

A method for preparing D-valine from L-valine by racemization and chemical resolution is presented. The resolving reagent, D-2, 3 -dibenzoyl tartaric acid was obtained by hydrolyzation of D-2, 3-dibenzoyl tartaric anhydride prepared by reaction of benzoyl chloride with D-tartaric acid. DL-valine was prepared by racemization of L-valine in the presence of aldehyde in a medium of acetic acid at 100 to 110 deg C for 3 h. In the presence of mineral acid, reaction of D-2, 3 -dibenzoyl tartaric acid with DL-valine formed diastreroisomeric salts at 84 to 95 deg C. Salt composed of D-2, 3 -dibenzoyl tartaric acid and D-valine precipitated when the diastreroisomeric salts mixtures were cooled to 15 deg C. The salt was reacted with base giving D-valine with yield of 70 percent to 80 percent and optical purity of over 98 percent.
机译:提出了一种通过外消旋和化学拆分从L-缬氨酸制备D-缬氨酸的方法。通过水解由苯甲酰氯与D-酒石酸反应制得的D-2,3-二苯甲酰基酒石酸酐,得到拆分试剂D-2,3-二苯甲酰基酒石酸。 DL-缬氨酸是通过在乙酸中,在醛存在下,将L-缬氨酸在100-110℃下外消旋3小时制得。在无机酸的存在下,D-2、3-二苯甲酰酒石酸与DL-缬氨酸的反应在84至95℃下形成非对映异构盐。由D-2、3-二苯甲酰酒石酸和D-缬氨酸组成的盐在沉淀时沉淀。将非对映异构盐混合物冷却至15℃。使盐与碱反应,得到D-缬氨酸,产率为70-80%,光学纯度超过98%。

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