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目的合成米诺膦酸。方法以2氨基吡啶和顺丁烯二酸酐为起始原料,经环合、酯化、氯代、还原和水解反应得到关键中间体2(咪唑并[1,2 a]吡啶3基)乙酸盐酸盐,该中间体再与亚磷酸反应后得到目标产物米诺膦酸。结果目标化合物的总收率为21.4%,其结构经MS、1H-NMR、13C-NMR、IR确证,高效液相色谱测得终产物的的纯度质量分数大于99.9%。结论该合成工艺简化了操作,降低了合成成本,适合于工业化生产。
Aim To synthesize minodronic acid. Methods 2-aminopyridine and maleic anhydride were used as starting materials to obtain the key intermediate 2 (imidazo [1,2-a] pyridin-3yl) acetate by cyclization, esterification, chlorination, reduction and hydrolysis. Acid salt, which is then reacted with phosphorous acid to obtain the target product minodronic acid. Results The total yield of the target compound was 21.4%. The structure was confirmed by MS, 1H-NMR, 13C-NMR and IR. The purity of the final product was more than 99.9% by HPLC. Conclusion The synthesis process simplifies the operation, reducing the cost of synthesis, suitable for industrial production.