二氧硫脲制备2,3-二氨基苯甲酰胺工艺研究  

Study on Reduction of 2,3-Diaminobenzoylamide by Thiourea Dioxide

作　　者：杜培 孙雅泉 Du Pei;Sun Yaquan(Yancheng Emergency Management Service Center,Jiangsu,224005)

机构地区：[1]盐城市应急管理服务中心,江苏224005

出　　处：《当代化工研究》2025年第5期169-171,共3页Modern Chemical Research

摘　　要：2,3-二氨基苯甲酰胺是合成抗肿瘤药物维利帕尼(Veliparib)的重要中间体。利用二氧化硫脲还原2-氨基-3-硝基苯甲酰胺成功地制备了2,3-二氨基苯甲酰胺。经对溶剂、温度和二氧硫脲用量优化,发现最佳工艺条件为:2-氨基-3-硝基苯甲酰胺、二氧化硫脲、氢氧化钠的摩尔比为1:5:10、溶剂为乙醇/水体积比为1:3、反应温度为70℃。反应温和,避免了高危工艺,收率高,产品纯度。目标产物的结构用IR、HRMS、1HNMR和13CNMR表征。2,3-diaminobenzamide is the key intermediate of Veliparib,an antitumor drug.2,3-diaminobenzamide was successfully prepared by reducing 2-amino-3-nitrobenzamide with thiourea dioxide.After optimizing the solvent,temperature,and dosage of thiourea,it was found that the optimal process conditions were as follows:the molar ratio of 2-amino-3-nitrobenzamide,thiourea dioxide,and sodium hydroxide was 1:5:10,the solvent was ethanol/water volume ratio was 1:3,and the reaction temperature was 70℃.High-risk process was avoided and the reaction was mild with high yield and high product purity.The structure of the target product was characterized by IR,HRMS,1HNMR and 13CNMR.

关 键 词：二氧硫脲 2-氨基-3硝基苯甲酰胺 硝基还原 2 3-二氨基苯甲酰胺 

分 类 号：TQ423.2[化学工程]