Synthesis of Isotope Labeled Protocatechuic Acid-(13COOH)
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 w...
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| Format: | Article |
| Language: | zho |
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Editorial Board of Journal of Isotopes
2020-12-01
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| Series: | Journal of Isotopes |
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| Online Access: | http://www.tws.org.cn/CN/abstract/abstract1823.shtml |
| Summary: | 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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| ISSN: | 1000-7512 1000-7512 |