1232431-11-6

基本信息
2-氨基-5-溴-4-甲氧基吡啶
2-氨基-4-甲氧基-5-溴吡啶
5-broMo-4-Methoxypyridin-2-aMine
2-Pyridinamine, 5-bromo-4-methoxy-
5-Bromo-4-methoxy-2-pyridinamine hydrobromide
物理化學性質(zhì)
制備方法

10201-73-7

1232431-11-6
步驟3:5-溴-4-甲氧基-2-氨基吡啶的合成 向4-甲氧基-2-氨基吡啶(12.4 g,100 mmol)的乙腈(500 mL)溶液中分批加入N-溴代丁二酰亞胺(17.8 g,100 mmol),反應(yīng)在0℃下進行并持續(xù)攪拌。加料完畢后,將反應(yīng)混合物在室溫下繼續(xù)攪拌1小時。反應(yīng)完成后,通過旋轉(zhuǎn)蒸發(fā)去除溶劑,殘余物用二氯甲烷溶解。所得溶液用飽和碳酸氫鈉溶液洗滌,有機相經(jīng)無水硫酸鈉干燥后濃縮,得到5-溴-4-甲氧基-2-氨基吡啶(20.3 g,收率100%),產(chǎn)物無需進一步純化即可用于后續(xù)反應(yīng)。質(zhì)譜(ESI)m/z:203.0 [M + H]+。
參考文獻:
[1] Patent: EP2952510, 2015, A1. Location in patent: Paragraph 0143
[2] Tetrahedron Letters, 2014, vol. 55, # 36, p. 5058 - 5061
[3] Patent: US2015/166505, 2015, A1. Location in patent: Paragraph 0428; 0429; 0450
[4] Patent: CN104513257, 2017, B. Location in patent: Paragraph 0411; 0412; 0413
[5] Patent: WO2012/58125, 2012, A1. Location in patent: Page/Page column 139; 140