CAS: 70374-37-7; Methyl 5-Chloro-3-(N-Methylsulfamoyl)Thiophene-2-Carboxylate

上下游产品

methanol

甲醇,在 三乙胺体系中,化学反应 2.0H,以93.3%的收率获得产物5-氯-3-(N-甲基氨磺酰基)-噻吩-2-甲酸甲酯
参考文献:氯诺昔康中间体5-氯-3-甲基磺酰胺噻吩-2-羧酸甲酯的合成方法
标题:氯诺昔康中间体5-氯-3-甲基磺酰胺噻吩-2-羧酸甲酯的合成方法
摘要:本发明属于药物合成技术领域,具体涉及一种氯诺昔康中间体5‑氯‑3‑甲基磺酰胺噻吩‑2‑羧酸甲酯的合成方法.以5‑氯‑3‑甲基磺酰胺噻吩‑2‑羧酸为起始原料,二氯甲烷作为反应溶剂,N,N‑二甲基甲酰胺为催化剂,氯化亚砜为氯代试剂,反应反应生成酰氯活性中间体,然后加入三乙胺和甲醇反应反应生成5‑氯‑3‑甲基磺酰胺噻吩‑2‑羧酸甲酯.本发明利用氯化亚砜为氯代试剂,避免了传统工艺中五氯化磷这一含磷试剂的使用,工艺更加环保;同时用二氯甲烷代替了高毒性的氯仿作作为反应溶剂,进一步降低了工艺对于环境的污染.

专利信息

专利号:US-11697658-B2
优先权日:2020-12-25
标题:Method for preparing lornoxicam
发明人：LIU ZHEN; XING DONGYE; ZHANG ZHONGZHENG; LI JIE; Han Yangong; CUI YALI; WANG LIRU; LIU HONGLIANG; MI YAN; LI LI; TANG JINGANG; KANG YI
权利人:BEIJING JINCHENG TAIER PHARMACEUTICAL CO LTD
摘要:The present disclosure relates to the technical field of drug synthesis, in particular to a method for preparing lornoxicam. The method includes the following steps: using 6-chloro-4-hydroxy-2-methyl-2-H-thieno[2,3-e]-1,2-thiazine methyl carboxylate-1,1-dioxide and 2-aminopyridine as raw materials, and xylene as a solvent; mixing the raw material and solvent, and adding a stabilizer, to obtain a mixture; subjecting the mixture to an ammonolysis; cooling the resulting reactant; conducting a vacuum concentration to remove the solvent; adding an organic solvent and slurrying, and filtering, to obtain a crude lornoxicam; and refining the crude lornoxicam to obtain the lornoxicam. In the present disclosure, p-toluenesulfonic acid is used as a stabilizer to reduce the reaction temperature and promote the reaction to proceed forward, thereby improving the quality and yield of the product.