945954-94-9

基本信息
methyl 6-bromo-3-methoxypyridine-2-carboxylate
2-Pyridinecarboxylic acid, 6-bromo-3-methoxy-, methyl ester
物理化學性質(zhì)
制備方法

321601-48-3

74-88-4

945954-94-9
以6-溴-3-羥基吡啶-2-甲酸甲酯和碘甲烷為原料合成6-溴-3-甲氧基吡啶甲酸甲酯的一般步驟:將6-溴-3-羥基吡啶-2-甲酸甲酯(4g,17.2mmol)、碘甲烷(7.15g,34.5mmol)和碳酸鉀(4.76g,34.5mmol)溶于N,N-二甲基甲酰胺(50mL)中,室溫攪拌反應3小時。反應完成后,減壓濃縮反應混合物,用水稀釋后,以乙酸乙酯(50mL×3)萃取。合并有機層,用無水硫酸鈉干燥,減壓濃縮,得到粗產(chǎn)物6-溴-3-甲氧基吡啶甲酸甲酯(4g,收率:90%)。產(chǎn)物經(jīng)核磁共振氫譜(CDCl3, 400MHz)鑒定:δ7.56(d,J = 8.0Hz,1H),7.25(d,J = 8.0Hz,1H),3.94(s,3H),3.90(s,3H)。質(zhì)譜(M + H)+:256/258。
參考文獻:
[1] Patent: WO2014/121418, 2014, A1. Location in patent: Page/Page column 45
[2] Patent: EP3255042, 2017, A2. Location in patent: Paragraph 0180; 0183
[3] Patent: WO2007/89031, 2007, A1. Location in patent: Page/Page column 84-85
[4] Patent: WO2014/209727, 2014, A1. Location in patent: Page/Page column 39
[5] Patent: WO2014/205593, 2014, A1. Location in patent: Page/Page column 41; 42