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目的设计并合成3,6-双羧甲基-4-氨基-6H-噻吩并[2,3-B]吡咯-2-羧酸。方法以柠檬酸为起始原料,经氧化酯化、Gewald反应、氮取代、环合、水解、脱羧反应制备得到目标化合物。结果合成了目标化合物,并利用质谱和核磁数据确证了结构;HPLC归一化法测得质量分数为96.98%。目标化合物的总收率为2.7%。结论 3,6-双羧甲基-4-氨基-6H-噻吩并[2,3-B]吡咯-2-羧酸的合成为雷奈酸锶中杂质的研究提供了方便。
Aim To design and synthesize 3,6-biscarboxymethyl-4-amino-6H-thieno [2,3-b] pyrrole-2-carboxylic acid. Methods Starting from citric acid, the target compound was prepared by oxidative esterification, Gewald reaction, nitrogen substitution, cyclization, hydrolysis and decarboxylation. Results The target compounds were synthesized and confirmed by MS and NMR. The mass fraction was 96.98% by HPLC. The total yield of the target compound was 2.7%. Conclusion The synthesis of 3,6-dicarboxymethyl-4-amino-6H-thieno [2,3-b] pyrrole-2-carboxylic acid provides convenience for the study of impurities in strontium ranelate.