866775-09-9

基本信息
3-氨基-6-溴吡啶-2-羧酸甲酯
3-氨基-6-溴吡啶-2-甲酸甲酯
methyl 3-amino-6-bromopyridine-2-carboxylate
3-AMINO-6-BROMOPYRIDINE-2-CARBOXYLIC ACID METHYL ESTER
2-Pyridinecarboxylic acid, 3-aMino-6-broMo-, Methyl ester
物理化学性质
制备方法

36052-27-4

866775-09-9
步骤2:将3-氨基吡啶-2-羧酸甲酯(17g,111.8mmol)溶于水(288mL)和2M硫酸(58mL)的混合溶剂中,室温下搅拌至完全溶解。随后,缓慢滴加溴(5.76mL,111.8mmol)的乙酸(43mL)溶液,滴加完毕后继续在室温下搅拌反应4小时。反应完成后,用2N氢氧化钠水溶液调节反应混合物的pH至6。用乙酸乙酯(每次等量)萃取水相两次,合并有机层并用无水硫酸钠干燥。减压蒸发除去有机溶剂,得到粗产物。粗产物通过硅胶柱色谱法纯化,以二氯甲烷为洗脱剂,得到3-氨基-6-溴吡啶-2-羧酸甲酯(19.2g,产率74%)为白色固体。产物经1H-NMR(300MHz,CDCl3)表征:δ3.94(3H,s),5.81(2H,brs),6.93(1H,d,J = 8.72Hz),7.32(1H,d,J = 8.71Hz)。
参考文献:
[1] Patent: EP2975031, 2016, A1. Location in patent: Paragraph 1071
[2] Patent: WO2005/97805, 2005, A1. Location in patent: Page/Page column 54
[3] Patent: US2015/57260, 2015, A1. Location in patent: Paragraph 0687; 0688
[4] Patent: WO2015/25026, 2015, A1. Location in patent: Page/Page column 164
[5] Patent: US2013/210819, 2013, A1. Location in patent: Paragraph 0252-0253