1266322-58-0

制備方法

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1266322-58-0
b) 7-溴喹啉-3-胺的合成:將2-(7-溴喹啉-3-基)異吲哚啉-1,3-二酮(10g,28.3mmol)懸浮于乙醇(200mL)中,加入肼(1.777mL,56.6mmol),隨后加熱回流1小時(shí)。反應(yīng)完成后,使混合物冷卻至室溫,收集沉淀并用少量乙醇洗滌。將濾液濃縮至干,得到灰色固體。將所得固體溶解于溫乙醇中,并吸附于硅膠上。通過硅膠柱色譜法(洗脫劑:50-100%乙酸乙酯/己烷梯度)純化,得到目標(biāo)化合物7-溴喹啉-3-胺(3.5g,收率56%)。1H NMR(400MHz,DMSO-d6)δ ppm:5.83(s,2H),7.14(d,J = 2.53Hz,1H),7.49(dd,J = 8.84, 2.02Hz,1H),7.54-7.65(m,1H),7.94(d,J = 1.77Hz,1H),8.46(d,J = 2.78Hz,1H)。
參考文獻(xiàn):
[1] Patent: WO2017/32840, 2017, A1. Location in patent: Page/Page column 265; 266
[2] Patent: WO2013/28447, 2013, A1. Location in patent: Page/Page column 117
[3] Patent: WO2013/52716, 2013, A1. Location in patent: Page/Page column 63
[4] Patent: WO2013/177253, 2013, A2. Location in patent: Page/Page column 64
[5] Patent: WO2014/8223, 2014, A2. Location in patent: Page/Page column 71-72