6311-47-3
6311-47-3 結(jié)構(gòu)式
基本信息
N-(5-bromo-2-nitrophenyl)benzenamine
BenzenaMine, 5-broMo-2-nitro-N-phenyl-
物理化學(xué)性質(zhì)
制備方法
321-23-3
62-53-3
6311-47-3
以2-氟-4-溴硝基苯和苯胺為原料合成5-溴-2-硝基-N-苯基-苯胺的一般步驟:將4-溴-2-氟硝基苯(5.6 g,20.9 mmol)和苯胺(2.5 g,72.2 mmol)溶于50 mL無(wú)水N-甲基吡咯烷酮(NMP)中。將反應(yīng)混合物加熱至110℃,攪拌反應(yīng)過(guò)夜。反應(yīng)完成后,冷卻至室溫,減壓蒸餾除去溶劑。粗產(chǎn)物通過(guò)硅膠柱色譜法純化,洗脫劑為環(huán)己烷/乙酸乙酯(9:1,v/v),得到橙色固體產(chǎn)物,收率為92%(5.7 g)。產(chǎn)物的1H-NMR(400 MHz,CD2Cl2)數(shù)據(jù)如下:δ= 9.48(s,1H),8.06(d,1H),7.46(t,2H),7.30(t,4H),6.89(d,1H)。
參考文獻(xiàn):
[1] Patent: WO2015/14944, 2015, A1. Location in patent: Page/Page column 115; 116
[2] Patent: WO2015/150203, 2015, A1. Location in patent: Page/Page column 85
[3] Patent: WO2014/100695, 2014, A1. Location in patent: Paragraph 00349
[4] Patent: US2015/30588, 2015, A1. Location in patent: Page/Page column 71
[5] Patent: US9295673, 2016, B2. Location in patent: Page/Page column 351; 352