723281-72-9

基本信息
3-硝基-4-氯-6-溴喹啉
6-溴-4-氯-3-硝基喹啉 100G
Quinoline, 6-broMo-4-chloro-3-nitro-
物理化學(xué)性質(zhì)
制備方法

853908-50-6

723281-72-9
步驟3:將6-溴-4-羥基-3-硝基喹啉(步驟2的產(chǎn)物,20 g,74.3 mmol)與三氯氧磷(POCl3,150 mL,1613 mmol)混合,攪拌反應(yīng)45分鐘。反應(yīng)完成后,將混合物冷卻至室溫,并緩慢倒入冰水中以淬滅反應(yīng)。通過(guò)過(guò)濾收集析出的固體,用冰冷的水洗滌,隨后將固體溶解于二氯甲烷(CH2Cl2)中。有機(jī)層用冷的飽和食鹽水洗滌,并用無(wú)水硫酸鈉(Na2SO4)干燥。減壓蒸發(fā)除去溶劑,得到6-溴-4-氯-3-硝基喹啉。產(chǎn)量:8 g(38%);1H NMR(CDCl3,500 MHz):δ 9.275(s,1H),8.611-8.615(d,1H,J = 2 Hz),8.100-8.118(d,1H,J = 9 Hz),8.026-8.048(dd,1H,J = 8.5 Hz,2 Hz)。
參考文獻(xiàn):
[1] Patent: US2015/320727, 2015, A1. Location in patent: Paragraph 0555; 0556
[2] Patent: WO2015/145369, 2015, A1. Location in patent: Page/Page column 38
[3] Patent: WO2009/155527, 2009, A2. Location in patent: Page/Page column 142
[4] MedChemComm, 2016, vol. 7, # 2, p. 297 - 310
[5] Patent: CN108456165, 2018, A. Location in patent: Paragraph 0047; 0081-0082