Synthesis of Isotope Labeled Protocatechuic Acid-(13COOH)
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Abstract
A novel synthesis method of protocatechuic acid-(13COOH) was designed. 3,4-dimethoxy bromobenzene as raw material, Grignard reagent was prepared by Grignard reaction, then passed through the 13C labeled 13CO2 gas, the intermediate 3,4-dimethoxy benzoic acid-(13COOH) was prepared. The crude product was obtained viademethylation with BBr3, which was decolorizing by activated carbon. Protocatechuic acid-(13COOH) was obtained by cooling crystallization. Synthesis route had the advantages of simple operation, short process flow, less side product, the yield was more than 45%, 13C labeled isotope abundance was not diluted. The product was characterized by HPLC, MS, 1H NMR and 13C NMR, the chemical purity was more than 99%, 13C enrichment was more than 98%. As an important tracer, it can provide a basis for medical and chemical research.
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