947249-13-0

基本信息
5-溴-3-(二氟甲氧基)吡啶-2-胺
5-bromo-3-(difluoromethoxy)-2-Pyridinamine
5-Bromo-3-(difluoromethoxy)pyridin-2-amine
5-bromo-3-(difluoromethoxy)pyridine-2-amine
2-Pyridinamine, 5-bromo-3-(difluoromethoxy)-
物理化學(xué)性質(zhì)
常見問題列表

947249-14-1

947249-13-0
以3-(二氟甲氧基)吡啶-2-胺為原料合成2-氨基-3-(二氟甲氧基)-5-溴吡啶的一般步驟:在0℃下,將N-溴代琥珀酰亞胺(2.61g,14.65mmol)在3分鐘內(nèi)緩慢加入至3-(二氟甲氧基)吡啶-2-胺(2.3g,14.36mmol)的乙腈溶液(15mL)中。反應(yīng)混合物在相同溫度下繼續(xù)攪拌20分鐘。隨后,將反應(yīng)液真空濃縮至干,所得粘性物質(zhì)用水稀釋,并用乙酸乙酯(3×60mL)萃取。合并有機(jī)層,用無水硫酸鈉干燥,再次濃縮至干。通過柱層析(硅膠,100-200目,20%乙酸乙酯的己烷溶液作為洗脫劑)純化殘余物,得到目標(biāo)產(chǎn)物5-溴-3-(二氟甲氧基)吡啶-2-胺(3.2g,收率93%)。產(chǎn)物經(jīng)核磁共振氫譜(400 MHz,DMSO-d6)確認(rèn):δ7.89(s,1H),7.51(s,1H),7.16(t,J = 73.6Hz,1H),6.34(s,2H)。
參考文獻(xiàn):
[1] Patent: WO2014/111496, 2014, A1. Location in patent: Page/Page column 108; 109
[2] Patent: WO2015/91889, 2015, A1. Location in patent: Page/Page column 74, 75
[3] Patent: US2015/175619, 2015, A1. Location in patent: Paragraph 0221; 0222
[4] Patent: WO2009/16460, 2009, A2. Location in patent: Page/Page column 56
[5] Patent: US2013/210818, 2013, A1. Location in patent: Paragraph 0416