55876-84-1

基本信息
THYL-5-BROMOMETHYLPYRIDINE-2-CARBOXYLATE
5-Bromomethyl-2-(1-methoxy-vinyl)-pyridine
METHYL-5-BROMOMETHYLPYRIDINE-2-CARBOXYLATE
5-(Bromomethyl)pyridine-2-carboxylic acid methyl ester
2-Pyridinecarboxylic acid, 5-(bromomethyl)-, methyl ester
物理化學(xué)性質(zhì)
制備方法

29681-38-7

55876-84-1
以5-甲基吡啶-2-羧酸甲酯為原料合成5-溴甲基吡啶-2-甲酸甲酯的一般步驟:在500mL圓底燒瓶中,將N-溴代琥珀酰亞胺(NBS,14.13g,79.38mmol,1.20當(dāng)量)和偶氮二異丁腈(AIBN,217mg,1.32mmol,0.02當(dāng)量)加入到5-甲基吡啶-2-羧酸甲酯(10g,66.15mmol,1.00當(dāng)量)的四氯化碳(CCl4,200mL)溶液中。將反應(yīng)混合物在80℃下攪拌16小時(shí)。反應(yīng)完成后,將混合物減壓濃縮。殘余物通過硅膠柱色譜法純化,采用乙酸乙酯/石油醚(5%至25%梯度)作為洗脫劑,得到5-溴甲基吡啶-2-甲酸甲酯(9.6g,57%收率),為黃色固體。質(zhì)譜(MS):m/z = 229.9 [M + H]+。
參考文獻(xiàn):
[1] Patent: US2016/96834, 2016, A1. Location in patent: Paragraph 0328
[2] Patent: WO2007/22371, 2007, A2. Location in patent: Page/Page column 90
[3] Patent: WO2012/80221, 2012, A1. Location in patent: Page/Page column 84
[4] Patent: US2013/274260, 2013, A1. Location in patent: Paragraph 0622-0623
[5] Patent: WO2013/3505, 2013, A1. Location in patent: Page/Page column 58