五氯柳胺合成工艺改进

Improved Synthesis of Oxyclozanide

以2,4-二氯-6-硝基苯酚为原料,依次通过催化加氢还原,与3,5,6-三氯水杨酸酰氯缩合,并在甲醇/水中加入还原性脱色剂精制得到五氯柳胺。总收率由原来的54.8%提高至89.6%,纯度达99.9%(HPLC测得)。产物结构经~1H NMR、元素分析及MS进行了表征。

Oxyclozanide was prepared from 2,6-dichloro- 4 -nitrophenol via catalytic hydrogenation, condensation with 3 , 5 , 6-trichlorosalicylryl chloride , and finally purification by reductive decoloring agent in methanol. The overall yield of oxiconazole nitrate was increased from 54.8% to 89.6 %, with a purity of 99.9%. The structures of the products were characterized by 1H NMR（MS spectra and organic elemental analysis.