摘要
本文报道一种未见文献报道的化合物2-氨基-N,3-二甲基-5-硫氰基苯甲酰胺的合成。从3-甲基氨茴酸出发,用两种不同方法得到2-氨基-N,3-二甲基苯甲酰胺,随后在0-5℃条件下与硫氰酸钠与溴素的混合物反应,高收率地得到2-氨基-N,3-二甲基5-硫氰基-苯甲酰胺。该化合物经核磁共振氢谱、碳谱、红外光谱和高分辨质谱表征和确认。同时考察了硫氰酸钠与溴素的用量及比例对反应产物纯度和收率的影响,发现2-氨基-N,3-二甲基苯甲酰胺、硫氰酸钠与溴素的摩尔比为1∶4∶2时,能以好的分离收率得到目标产物。
The synthesis of a novel compound 2-amino-N,3-dimethyl-5-thiocyanatobenzamide was reported in this article. Treatment of 3-methylanthranilic acid by two different approaches afforded 2-amino-N,3-dimethylbenzamide. This intermediate product was reacted with the mixture of sodium thiocyanate and bromine at 0-5℃ to get 2-amino-N,3-dimethyl-5-thiocyanatobenzamide with good yield. The target compound was characterized and confirmed by1 H NMR,13 C NMR,IR and ESI-HRMS. The influence of stoichiometry and the ratio of sodium thiocyanate and bromine on the purity and yield of product was investigated.When the molar ratio of 2-amino-N,3-dimethylbenzamide,sodium thiocyanate and bromine was 1 ∶ 4 ∶ 2,the target product was obtained with good isolated yield.
出处
《化学研究与应用》
CAS
CSCD
北大核心
2015年第11期1746-1750,共5页
Chemical Research and Application
基金
安阳市锐普农化有限责任公司项目资助
