A kind of method for splitting and preparing optically pure r-1-phenethylamine

Abstract

The invention relates to a method for preparing R-1-phenethylamine through dynamic kinetic resolution. Using 1‑phenethylamine as raw material, Novozym 435 as resolution catalyst, D‑(‑)‑O‑acetylmandelic acid as acyl donor, KT‑02 (nickel catalyst) as racemization catalyst, in autoclave 1-Phenylethylamine is completely converted to obtain (R)-(1-Phenylethyl)acetamide (ee value 99%); acidolysis is carried out after purification of the amide to obtain R-1-Phenylethylamine Salt, the salt is then subjected to operations such as alkalization, extraction, drying, and concentration to obtain R-1-phenylethylamine, and the product yield and ee value of the whole step can reach more than 90%. The invention has the characteristics of cheap and easy-to-obtain racemization catalyst, complete utilization of raw materials, good product yield, high purity and the like. In the production and preparation of R-1-phenethylamine, it has great guidance and application value.

Description

technical field [0001] The invention relates to a resolution and preparation method of optically pure chiral amine, in particular to a resolution and preparation method of optically pure R-1-phenylethylamine. Background technique [0002] Optically pure chiral amines are very important pharmaceutical intermediates. At present, optically pure chiral amines are mainly obtained through the following methods: enzymatic resolution (Indian J. Chem. Sect. B 2005, 44, 1312-1316; J. Org. Chem. 1997, 62, 3488-3495); Chemical resolution: resolution with chiral α-hydroxyphenylacetic acid (US6342636; Tetrahedron: asymmetry, 1998, 9, 2219-2212) or protected chiral glycerol derivatives (Tetrahedron: asymmetry, 1996, 7, 1117-1122 ; Tetrahedron: asymmetry, 2002,13, 2277-2282); obtained by asymmetric synthesis of the corresponding aldehyde (WO2004 / 110976; J. Org. Chem.1992, 57, 1237-1241). [0003] Among the existing methods, the cost of asymmetric synthesis is high and it is often difficul...

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Problems solved by technology

[0003] Among the existing methods, the cost of asymmetric synthesis is high and it is often difficult to obtain products with high optical purity; chemical resolution and enzymatic kinetic resolution have the disadvantage of low raw material utilization, which is only 50% at most; In the reported enzymatic dynamic kinetic resolution method, the racemization catalysts used are usually complexes of noble metals such as ruthenium and rhodium. The cost of these racemization catalysts is extremely high. Although some methods achieve high conversion rates, the products are difficult Achieve Satisfactory Optical Purity

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