阿那曲唑的合成工艺改进研究  

Improvement of the synthetic method of anastrozole

作　　者：王立升[1] 郭大涛[1] 李钰[1] 杨华[1] 周永红[1] 

机构地区：[1]广西大学化学化工学院,广西南宁530004

出　　处：《化学试剂》2012年第7期662-664,共3页Chemical Reagents

基　　金：教育部留学人员科研启动基金(教外司留[2007]1108号)

摘　　要：以3,5-二溴甲苯为原料,经插羰、甲基化、氯代、氰代、溴代、N-烷基化6步反应合成标题化合物,考察了不同催化剂、反应时间、反应温度等因素对反应结果的影响,选择了氢化钠作为合成目标产物的缚酸剂,避免了同分异构体的产生。确定最佳工艺条件为:以PdCl2(PPh3)2作催化剂,Et3N做碱,90℃,9.12×106Pa为反应条件,获得了较好结果,总收率55.2%。产物结构经1HNMR和MS确证,改进后的合成方法简便,适合工业化生产。Anastrozole was synthesized via six reaction steps of carbonylation,methylation chlorination,cyanidation,bromination and N-alkylation using 3,5-Dibromotoluene as the starting material.The factorssuch as different catalysts,the reaction time and reaction temperature had been investigated.Sodium hydride was used as the bind acid agent to avoid the produce of the isomer.The reaction conditions were described as follows PdCl2（PPh3）2 as catalysts and Et3N as alkali,the reaction was heated at 90 ℃ under 9.12×106 Pa.The total yield was 55.2%.The structure of final product was confirmed by 1HNMR and MS.Compared with the methods in pafent,this method was more simple to operate with low cost and high yield and was also more suitable for the large scale production.

关 键 词：阿那曲唑 合成 3 5-二溴甲苯 

分 类 号：O621.3[理学—有机化学]