915006-52-9
915006-52-9 结构式
基本信息
5-氨基-2-溴-6-碘吡啶
3-AMino-6-broMo-2-iodopyridine
5-Amino-2-bromo-6-iodopyridine
3-PyridinaMine, 6-broMo-2-iodo-
6-BroMo-2-iodo-pyridin-3-ylaMine
5-Amino-2-bromo-6-iodopyridine ISO 9001:2015 REACH
物理化学性质
制备方法
13534-97-9
915006-52-9
以5-氨基-2-溴吡啶为原料合成5-氨基-2-溴-6-碘吡啶的一般步骤:向搅拌中的6-溴-吡啶-3-基胺(10.2g,0.0580mol)和Ag2SO4(18.1g,0.0580mol)在乙醇(150mL)中的溶液中加入碘(7.59g,0.0580mol),反应混合物搅拌过夜。随后,加入己烷(200mL),将混合物通过硅藻土过滤。在减压下除去溶剂,将残余物溶解于氯仿(200mL)中,依次用饱和硫代硫酸钠水溶液(100mL)和水(1×100mL)洗涤,并用无水硫酸钠干燥。减压浓缩溶剂,将残余物溶于热乙酸乙酯(100mL)中,过滤后加入己烷(100mL)处理。过滤得到白色结晶状产物5-氨基-2-溴-6-碘吡啶11.2g,收率65%。1H-NMR(CDCl3;400MHz):δ7.10(d,1H,J=8.2Hz),6.74(d,1H,J=8.2Hz),4.06(br s,2H)。
参考文献:
[1] Patent: US2007/249649, 2007, A1. Location in patent: Page/Page column 74
[2] Patent: US2007/249608, 2007, A1. Location in patent: Page/Page column 41
[3] Patent: WO2007/123516, 2007, A1. Location in patent: Page/Page column 109-110
[4] Patent: WO2009/149820, 2009, A1. Location in patent: Page/Page column 82-83
[5] Journal of Medicinal Chemistry, 2013, vol. 56, # 21, p. 8860 - 8871