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该文提出以1,3-二溴-5,5-二甲基海因作为溴化剂合成6-氨基-5-溴喹喔啉的方法。分别以1,3-二溴-5,5-二甲基海因、N-溴代丁二酰亚胺和液溴作为溴化剂,考察了温度、溶剂和反应时间对溴化反应的影响,确定了最佳反应条件:n(1,3-二溴-5,5-二甲基海因)∶n(6-氨基喹喔啉)=1.0∶2.0,反应温度20℃,以二氯甲烷为溶剂,反应时间2 h。在该反应条件下,5-溴-6-氨基喹喔啉的溴化收率达97.6%。该方法反应条件温和,步骤精简,无溴化杂质生成,并以高收率达到医用原料的要求。现已完成10 kg级扩试。
This paper proposes a method of synthesizing 6-amino-5-bromoquinoxaline with 1,3-dibromo-5,5-dimethylhydantoin as brominating agent. The effects of temperature, solvent and reaction time on the bromination reaction were investigated with 1,3-dibromo-5,5-dimethylhydantoin, N-bromosuccinimide and liquid bromine respectively The optimal reaction conditions were as follows: n (1,3-dibromo-5,5-dimethylhydantoin): n (6-aminoquinoxaline) = 1.0: 2.0, reaction temperature 20 ℃, Methane as solvent, reaction time 2 h. The bromination yield of 5-bromo-6-aminoquinoxaline was 97.6% under the reaction conditions. The method has the advantages of mild reaction conditions, streamlined steps, no brominated impurities generation, and high requirements for medical raw materials. Has now completed 10 kg-class expansion test.