美沙拉嗪的合成工艺改进

Improved Synthetic Process of Masalazine

以对硝基苯酚为起始原料,经Duff醛基化、在溴化铜/叔丁基过氧化氢/叔丁醇钾条件下氧化、氯化亚锡/浓盐酸体系中还原得到目标化合物美沙拉嗪,总收率为54%,化合物结构经IR、~1H NMR表征。在Duff醛基化反应过程中,采用对甲苯磺酸为催化剂,简化了操作,收率由文献的67%提高至93%。整条路线操作简单,适合工业化生产。

Masalazine in a total yield of 54% was obtained via three steps of improved Duff formylation,oxidization in presence of CuBr2/TBHP/t-BuOK,and reduction in the SnCl2/HCl system,from p-nitrophenol as starting material.The structures of intermediates and product were characterized by IR and 1H NMR.p-TSOH used in the process of Duff formylation not only simplified the operation steps,but also improved the yield to 93%,higher than that reported in the literature(67%).The whole route was easy to operate and suitable for industrial production.