【摘要】 以2-氨基-5-甲基吡啶为起始原料,经重氮化反应,水解后得到中间体2-羟基-5-甲基吡啶,在无水碳酸钾和碘化铜存在下与碘苯进行亲核取代反应,生成目标产物吡非尼酮,经工艺优化后反应总收率为66.6%,较文献报道收率提高了16.6%。终产物与中间体的结构经核磁共振氢谱、质谱确证。通过不同方法制备了吡非尼酮的三种不同晶型样品,改善了晶型的制备工艺,提出了新的晶型制备方法。采用粉末X射线衍射法、差示扫描量热法、红外光谱法对不同晶型进行了表征分析。更多还原

【Abstract】 Using 2-amino-5-methyl-pyridine as the starting material, 2-hydroxy-5-methyl-pyridine was obtained by diazotization and hydrolysis. Then, in the presence of anhydrous potassium carbonate and copper iodide, the reaction was carried out with iodobenzene to produce the target product named pirfenidone. The total yield of the reaction was 66.6%, this is an increase of 16.6% over that reported in the literature, and the structures of the final products and intermediates were confirmed by1 H NMR and EI-MS. Three forms of pirfenidone were prepared. The structure of the crystals was analyzed by powder X-ray diffraction(PXRD),differential scanning calorimetry(DSC) and the infrared spectrometry(IR).更多还原