N,N-二甲基-10H-2-吩噻嗪磺酰胺的合成  

Synthesis of N,N-Dimethyl-10H-phenothiazine-2-sulfonamide

作　　者：冯德日 李林森[1] 师秀艳[1] 冮岩[1] 范业明[1] 

机构地区：[1]沈阳医学院,辽宁沈阳110034

出　　处：《精细化工》2014年第7期862-865,共4页Fine Chemicals

摘　　要：以邻溴苯胺为起始原料,经缩合、水解、N,N-二甲基-3-硝基-4-氯苯磺酰胺缩合、锌粉还原、铜催化Ullmann反应,得到目标化合物。并考察了缩合反应不同溶剂、碱、反应温度,还原反应还原剂的用量,Ullmann反应催化剂的用量、反应时间、反应温度对反应收率的影响。优化后5步反应总收率可达45.5%,且反应条件温和,后处理简便,在该工艺的中试生产中4批样品的车间总收率分别为38.2%、36.7%、36.9%、38.5%,且产品质量可靠,稳定性良好,产品经ESI-MS和1HNMR确证结构。N,N-dimethyl-10H-phenothiazine-2-sulfonamide is the very important intermediate of Pipothiazine which is the representative drug of anti-psychotic disorders.In this study, o-bromoaniline was condensed and hydrolysesed , then condensed by N,N-dimethyl-4-chloro-3-nitrobenzenesulfonamide,and reduced by zinc dust,after via Ullmann reaction to give the final target compounds. The effects of different solvent/base、temperature on the yield of condensation,reducing agent proportion on the yield of the reduction,and catalyst agent proportion、reaction temperature and reaction time on the yield of the Ullmann reaction were studied.After 5 steps,the total yield could reach up to 45.5%, the reaction condition was mild,and easily to be treated,the structure of the targer compound was confirmed by means of ESI-MS and ^1HNMR.

关 键 词：哌泊噻嗪 N N-二甲基-10H-2-吩噻嗪磺酰胺 工艺研究 医药与日化原料 

分 类 号：TQ460.31[化学工程—制药化工]