85223-93-4

基本信息
4-溴-2,5-二甲基苯酚
4-Bromo-2,5-dimethylphenol
Phenol, 4-bromo-2,5-dimethyl-
4-Bromo-2,5-dimethylphenol98%
物理化學(xué)性質(zhì)
制備方法

95-87-4

85223-93-4
在室溫條件下,將四丁基三溴化銨(19.9g,41.39mmol)的氯仿(150mL)溶液緩慢滴加至攪拌中的2,5-二甲基苯酚(5.0g,40.9mmol)的水(150mL)懸浮液中。反應(yīng)混合物在室溫下持續(xù)攪拌2小時(shí)。反應(yīng)完成后,分離有機(jī)層,并用無(wú)水硫酸鈉干燥。干燥后的有機(jī)相經(jīng)過(guò)濾,減壓濃縮除去溶劑。所得粗產(chǎn)物通過(guò)硅膠柱層析進(jìn)行純化,洗脫劑為體積比1:5的己烷-乙酸乙酯混合溶劑,最終得到2,5-二甲基-4-溴苯酚,為棕色固體(6.2g,收率76%)。產(chǎn)物結(jié)構(gòu)經(jīng)1H NMR(300MHz,DMSO-d6)確認(rèn):δ 9.47(s,1H),7.24(s,1H),6.74(s,1H),2.21(s,3H),2.07(s,3H)。薄層色譜(TLC)分析條件:Uniplate硅膠板,厚度250微米;流動(dòng)相為體積比9:1的己烷-乙酸乙酯;Rf值為0.52。
參考文獻(xiàn):
[1] Tetrahedron, 2007, vol. 63, # 34, p. 8242 - 8249
[2] Letters in Organic Chemistry, 2018, vol. 15, # 8, p. 682 - 687
[3] Journal of the Chilean Chemical Society, 2011, vol. 56, # 4, p. 863 - 865
[4] Bulletin of the Chemical Society of Japan, 1987, vol. 60, # 11, p. 4187 - 4189
[5] Synthetic Communications, 2010, vol. 40, # 6, p. 868 - 876