881658-92-0

基本信息
8-溴-2-甲氧基-1,5-二氮雜萘
8-Bromo-2-methyloxy-1,5-naphthyridine
1,5-Naphthyridine, 8-broMo-2-Methoxy-
物理化學(xué)性質(zhì)
制備方法
![6-METHOXY-[1,5]-NAPHTHYRIDIN-4-OL](/CAS2/GIF/23443-25-6.gif)
23443-25-6

881658-92-0
以6-甲氧基-1,5-萘啶-4-醇(21.5 g)為原料,在氮氣保護下,將其溶解于DMF(150 mL)中,并在0℃下攪拌。緩慢滴加三溴化磷(13.5 mL),滴加完畢后,將反應(yīng)混合物逐漸升溫至室溫,繼續(xù)攪拌反應(yīng)90分鐘。反應(yīng)完成后,加入水(375 mL)淬滅反應(yīng),并用固體碳酸鈉調(diào)節(jié)pH至7。通過抽濾收集析出的固體產(chǎn)物,用燒結(jié)漏斗抽吸干燥2小時,隨后在45℃下真空干燥,得到目標(biāo)化合物8-溴-2-甲氧基-1,5-萘啶(26.0 g,收率90%)。產(chǎn)物經(jīng)1H-NMR(DMSO-d6)表征,化學(xué)位移(δ, ppm)如下:8.59(d, 1H),8.30(d, 1H),8.08(d, 1H),7.33(d, 1H),4.06(s, 3H)。
參考文獻(xiàn):
[1] Patent: EP2080761, 2009, A1. Location in patent: Page/Page column 15
[2] Patent: WO2010/81874, 2010, A1. Location in patent: Page/Page column 17-18
[3] Patent: US2006/223810, 2006, A1. Location in patent: Page/Page column 18
[4] Patent: WO2010/101949, 2010, A1. Location in patent: Page/Page column 125