67346-74-1
67346-74-1 結(jié)構(gòu)式
基本信息
3-乙炔吡啶-2-胺
3-乙炔基吡啶-2-胺
2-氨基-3-乙炔基吡啶
3-ethynylpyridin-2-aMine
3-Ethynyl-2-pyridinamine
2-Amino-3-ethynylpyridine
2-Pyridinamine, 3-ethynyl-
3-Ethynylpyridin-2-amine - [E45198]
物理化學(xué)性質(zhì)
制備方法
936342-23-3
67346-74-1
一般步驟:制備3-乙炔基吡啶-2-胺;向3-((三甲基硅烷基)乙炔基)吡啶-2-胺(28.1 g,148 mmol)的四氫呋喃(300 mL)溶液中加入四丁基氟化銨(1 M四氫呋喃溶液,20 mL,20 mmol),室溫?cái)嚢?5分鐘。反應(yīng)完成后,向反應(yīng)溶液中加入水,然后用乙酸乙酯萃取四次。合并有機(jī)層,用無水硫酸鈉干燥,減壓濃縮除去溶劑。殘余物通過硅膠柱色譜純化(洗脫劑:庚烷/乙酸乙酯=1:1,隨后調(diào)整為1:2),得到目標(biāo)產(chǎn)物3-乙炔基吡啶-2-胺(16.4 g,收率93.7%)。1H-NMR(DMSO-d6)δ(ppm):4.43(1H,s),6.14(2H,brs),6.53(1H,dd,J=4.8 Hz,7.2 Hz),7.53(1H,d,J=7.2 Hz),7.96(1H,d,J=4.8 Hz)。
參考文獻(xiàn):
[1] Patent: US2009/82403, 2009, A1. Location in patent: Page/Page column 51-52
[2] Patent: US2007/105904, 2007, A1. Location in patent: Page/Page column 53-54
[3] Patent: US2010/331282, 2010, A1. Location in patent: Page/Page column 11
[4] Chemistry - A European Journal, 2010, vol. 16, # 27, p. 7992 - 7995
[5] Patent: EP2065377, 2009, A1. Location in patent: Page/Page column 59