泼尼松的合成工艺改进

Improvement of Synthetic Process of Prednisone

针对泼尼松原有工艺路线长、选择性差、产物分离复杂等问题,提出了1条以11α,17α-二羟基孕甾-1,4-二烯-3,20-二酮为起始原料,经过碘代、亲核取代、氧化和水解4步反应得到泼尼松的工艺路线。结果表明,采用先碘代后氧化的方法,提升了碘代反应的区域选择性及卤代中间体的产品质量,路线经优化后总收率可达47.2%,产物结构经1H NMR、13CNMR及熔点等数据确认,该方法具有收率高、操作简单、产物易分离等优点。

Aiming at the the problems of long process route,poor selectivity and complex product separation of prednisone,a process route was proposed to obtain prednisone from 11α,17α-dihydroxypregnan-1,4-diene-3,20-dione through iodination,nucleophilic substitution,oxidation and hydrolysis.The results showed that the regional selectivity of iodination and the product quality of halogenated intermediates were improved by the method of first iodination and then oxidation.The total yield of the optimized route was up to 47.2%,and the structure of the product was confirmed by 1 H NMR,13C NMR and melting point data.The method has the advantages of high yield,simple operation and easy separation of products.