113118-81-3
37669-64-0
在0℃下,將硼氫化鈉(2.2 g,59.1 mmol)緩慢加入至5-溴吡啶-3-甲醛(10.0 g,53.7 mmol)的甲醇(100 mL)懸浮液中。反應(yīng)混合物在0℃下持續(xù)攪拌1小時,隨后通過緩慢加入水(5.0 mL)淬滅反應(yīng)。反應(yīng)完成后,通過旋轉(zhuǎn)蒸發(fā)儀除去溶劑,得到淺黃色油狀物。將此油狀物重新溶解于乙酸乙酯中,并用去離子水洗滌。有機層經(jīng)無水硫酸鈉干燥后,過濾并真空濃縮,得到3-溴吡啶-5-甲醇(9.6 g,收率95%),為無色油狀物。質(zhì)譜分析結(jié)果:188.0和190.0(M + H+)。
參考文獻(xiàn):
[1] Patent: WO2013/79452, 2013, A1. Location in patent: Page/Page column 143
[2] Patent: US2013/143863, 2013, A1. Location in patent: Paragraph 1076; 1077; 1078
[3] Journal of Medicinal Chemistry, 2016, vol. 59, # 10, p. 4913 - 4925
[4] Patent: US2013/267495, 2013, A1. Location in patent: Paragraph 0454-0455
[5] Patent: US2013/296302, 2013, A1. Location in patent: Paragraph 0549