116557-46-1

基本信息
3-溴-2-甲氧基苯胺
2-amino-6-bromoanisole
3-Bromo-2-methoxybenzenamine
BenzenaMine, 3-broMo-2-Methoxy-
3-bromo-2-methoxyphenylamine hydrochloride
2-Amino-6-bromoanisole, 3-Bromo-o-anisidine
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

98775-19-0

116557-46-1
以2-溴-6-硝基苯甲醚為原料合成3-溴-2-甲氧基苯胺的一般步驟如下:將1-溴-2-甲氧基-3-硝基苯(20.1g,86.6mmol)與鐵粉(33.4g,598mmol)在乙酸/水(1:1,600mL)的混合溶劑中加熱至80℃。反應(yīng)持續(xù)1.5小時(shí)后,將混合物冷卻至室溫并過(guò)濾。濾得的固體用乙酸乙酯和水分次洗滌。合并有機(jī)層,用飽和NaHCO3水溶液洗滌,無(wú)水硫酸鈉干燥后,減壓濃縮。殘余物通過(guò)柱色譜法(洗脫劑:石油醚/乙酸乙酯=20:1至10:1)純化,得到黃色固體3-溴-2-甲氧基苯胺(17.4g,產(chǎn)率99%)。1H-NMR(300MHz,DMSO-d6)δ(ppm):3.66(s,3H),5.23(s,2H),6.64-6.76(m,3H)。
參考文獻(xiàn):
[1] Patent: EP2987787, 2016, A1. Location in patent: Paragraph 0131
[2] Patent: WO2014/74661, 2014, A1. Location in patent: Paragraph 00173
[3] Patent: US2014/296229, 2014, A1. Location in patent: Paragraph 0258; 0259
[4] Patent: WO2014/154760, 2014, A1. Location in patent: Page/Page column 55-56
[5] Patent: WO2018/75937, 2018, A1. Location in patent: Paragraph 00487; 00495; 00496