845827-14-7
845827-14-7 結(jié)構(gòu)式
基本信息
2-broMo-5-(difluoroMethoxy)pyridine
Pyridine,2-bromo-5-(difluoromethoxy)-
物理化學(xué)性質(zhì)
制備方法
55717-45-8
1895-39-2
845827-14-7
以6-溴吡啶-3-醇(1.2g,6.9mmol)和二氟氯乙酸鈉(2.1g,13.8mmol)為原料,在無水DMF(10ml)中加入碳酸鉀(1.24g,8.97mmol),將混合物在80°C下攪拌反應(yīng)20小時(shí)。反應(yīng)完成后,冷卻至室溫,將反應(yīng)混合物在EtOAc和水之間分配。水層用EtOAc反萃取,合并有機(jī)相,用無水硫酸鈉干燥后濃縮。粗產(chǎn)物通過Redi-Sep預(yù)填充硅膠柱(40g)進(jìn)行色譜純化,采用0至10% EtOAc的己烷溶液梯度洗脫,得到2-溴-5-二氟甲氧基吡啶(0.89g,4.0mmol,收率58%),為無色油狀物。ESI-MS (M+1) m/z: 225.8。
參考文獻(xiàn):
[1] Journal of Medicinal Chemistry, 2010, vol. 53, # 23, p. 8421 - 8439
[2] Patent: US2013/225552, 2013, A1. Location in patent: Paragraph 0902
[3] Patent: EP1741703, 2007, A1. Location in patent: Page/Page column 73
[4] Patent: US2018/37594, 2018, A1. Location in patent: Paragraph 0280-0283
[5] Patent: US2014/249104, 2014, A1. Location in patent: Page/Page column
