337915-79-4

基本信息
4-溴-2-甲基氨基苯胺 10G
5-溴-N1-甲基-1,2-苯二胺
5-溴-1-N-甲基苯-1,2-二胺
4-Bromo-2-methylaminoaniline
5-Bromo-N1-methyl-1,2-benzenediamine
5-Bromo-N1-methylbenzene-1,2-diamine
4-Bromo-N2-methyl-1,2-benzenediamine
4-bromo-2-N-methylbenzene-1,2-diamine
4-bromo-N2-methyl-benzene-1,2-diamine
1,2-BENZENEDIAMINE, 4-BROMO-N2-METHYL-
1,2-BENZENEDIAMINE, 4-BROMO-N2-METHYL- ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
制備方法

302800-13-1

337915-79-4
以5-溴-N-甲基-2-硝基苯胺(350 mg,1.51 mmol)為原料,與鋅粉(495 mg,7.57 mmol)和氯化銨(810 mg,15.15 mmol)在甲醇(4 mL)和水(2 mL)的混合溶劑中,于室溫下攪拌反應(yīng)1小時(shí)。反應(yīng)完成后,通過(guò)過(guò)濾去除不溶物,濾液用飽和碳酸氫鈉溶液中和。隨后,將反應(yīng)混合物濃縮,并用乙酸乙酯萃取。分離有機(jī)層,依次用水和飽和食鹽水洗滌,經(jīng)無(wú)水硫酸鎂干燥后,減壓濃縮,得到4-溴-2-甲基氨基苯胺,為棕色固體(282 mg,收率93%)。產(chǎn)物經(jīng)1H NMR(400 MHz,DMSO-d6)確認(rèn):δ 2.68(3H,d,J = 4.9 Hz),4.60(2H,s),4.87(1H,d,J = 4.9 Hz),6.32-6.58(3H,m)。質(zhì)譜(ESI/APCI)顯示m/z = 202.09 [M + H]+。
參考文獻(xiàn):
[1] Bioorganic and Medicinal Chemistry, 2016, vol. 24, # 11, p. 2486 - 2503
[2] Patent: CN108689942, 2018, A. Location in patent: Paragraph 0463; 0468-0469
[3] Patent: WO2012/174312, 2012, A2. Location in patent: Page/Page column 216-217
[4] Patent: WO2008/82487, 2008, A2. Location in patent: Page/Page column 111-112
[5] Patent: WO2004/111036, 2004, A1. Location in patent: Page 21