941294-54-8

基本信息
5-溴-2-甲氧基氰吡啶
5-溴-3-氰基-2-甲氧基吡啶
5-溴-2-甲氧基-3-氰基吡啶
3-Bromo-5-cyano-6-methoxypyridine
5-Bromo-2-methoxynicotinonitrile98%
5-bromo-2-methoxypyridine-3-carbonitrile
5-Bromo-2-methoxy-3-pyridinecarbonitrile
3-Pyridinecarbonitrile, 5-bromo-2-methoxy-
5-Bromo-2-methoxypyridine-3-carbonitrile, 5-Bromo-3-cyano-2-methoxypyridine
物理化学性质
安全数据
制备方法

7254-34-4

941294-54-8
以3-氰基-2-甲氧基吡啶为原料合成5-溴-3-氰基-2-甲氧基吡啶的一般步骤:在0℃条件下,将12.23 g(149 mmol)乙酸钠和7.66 mL(149 mmol)溴逐滴加入至含有10 g(74.6 mmol)3-氰基-2-甲氧基吡啶的29 mL乙酸溶液中。反应混合物随后在70℃下加热反应过夜。反应完成后,将反应体系冷却至室温,并倒入冰浴中。通过过滤收集析出的固体产物,用水充分洗涤,并于50℃下干燥,最终得到11.6 g(产率73%)目标化合物5-溴-3-氰基-2-甲氧基吡啶,为白色固体。产物经LC-MS(EI, m/z)分析确认:(M+1) 214.95。1H NMR(400 MHz, DMSO-d6)δ: 8.61(1H, d, J = 2.4 Hz, Ar-H), 8.60(1H, d, J = 2.4 Hz, Ar-H), 3.98(3H, s, OCH3)。
参考文献:
[1] Patent: WO2012/101239, 2012, A1. Location in patent: Page/Page column 55
[2] Patent: US2013/85144, 2013, A1. Location in patent: Paragraph 0281; 0282; 0283
[3] Patent: EP2689778, 2014, A1. Location in patent: Paragraph 0185
[4] Patent: WO2014/16433, 2014, A1. Location in patent: Page/Page column 54
[5] Patent: WO2014/16434, 2014, A1. Location in patent: Page/Page column 53-54