99455-15-9
99465-10-8
以7-溴-2-氯喹啉為原料合成7-溴喹啉-2(1H)-酮的一般步驟如下:將7-溴-2-氯喹啉(5.0g,20.6mmol)溶于5M鹽酸水溶液(133mL)和1,4-二惡烷(14mL)的混合溶劑中,攪拌并加熱回流2小時(shí)。反應(yīng)完成后,冷卻至室溫,過濾收集析出的沉淀,用去離子水洗滌,得到7-溴喹啉-2(1H)-酮,為無(wú)色固體(4.3g,收率93%)。產(chǎn)物經(jīng)1H NMR(400MHz,DMSO-d6)表征:δ11.80(s,1H),7.91(d,J=8.0Hz,1H),7.63(d,J=8.0Hz,1H),7.48(d,J=8.0Hz,1H),7.34(dd,J=8.0,4.0Hz,1H),6.53(d,J=4.0Hz,1H)。
參考文獻(xiàn):
[1] Patent: US2015/210655, 2015, A1. Location in patent: Paragraph 0291
[2] Patent: US9522894, 2016, B2. Location in patent: Page/Page column 34
[3] Patent: WO2008/71961, 2008, A1. Location in patent: Page/Page column 103-104
[4] Patent: WO2006/134378, 2006, A1. Location in patent: Page/Page column 61-62