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目的:设计简便、经济的合成路线,制备2-(3-氰基-4-异丁氧基苯基)-4-甲基-5-噻唑甲酸(Fe-buxostat)。方法:以对氰基苯酚为起始原料,经硫化氢解、环合、甲酰化、烷基化成醚、醛基肟化脱水成氰基、酯水解、酸化得到Febuxostat。结果:总收率26%,结构经核磁共振氢谱(1H-NMR)、质谱(MS)、元素分析(EA)和红外(IR)确证,含量99.8%以上(HPLC归一化法测定)。结论:该新合成路线中原料价廉易得、操作简便,适合工业化生产。
OBJECTIVE: To design a convenient and economical synthetic route to prepare 2- (3-cyano-4-isobutoxyphenyl) -4-methyl-5-thiazolecarboxylic acid (Fe-buxostat). Methods: The p-cyanophenol was used as the starting material, which was subjected to hydrogenation, cyclization, formylation and alkylation to form ether. The aldehyde was deaminated to form a cyano group through oximation, and the ester was hydrolyzed and acidified to obtain Febuxostat. Results: The total yield was 26%. The structure was confirmed by 1H-NMR, MS, EA and IR. The content was over 99.8% (HPLC normalization method). Conclusion: The raw materials in the new synthetic route are cheap and easy to operate, and are suitable for industrialized production.