52311-50-9

物理化學(xué)性質(zhì)
制備方法

23056-36-2

141-52-6

52311-50-9
一般步驟:在0℃條件下,將2-氯-4-硝基吡啶(170g,1070mmol)的THF(2L)溶液緩慢加入乙醇鈉(109.45g,1610mmol)中。反應(yīng)混合物在25℃下攪拌12小時(shí)。通過(guò)LCMS和TLC(展開(kāi)劑:石油醚/乙酸乙酯=5:1,Rf=0.6)監(jiān)測(cè)反應(yīng)完成。反應(yīng)完成后,過(guò)濾混合物,濾液在減壓下濃縮以除去大部分溶劑。殘余物用乙酸乙酯(800mL×3)萃取,有機(jī)層用飽和氯化鈉溶液(1L)洗滌,無(wú)水硫酸鈉干燥,濃縮后得到2-氯-4-乙氧基吡啶(157g,1.0mol,收率92%)為固體。1H NMR(400MHz,CD3OD)δ8.15(d,J=6.0Hz,1H),6.99(d,J=2.0Hz,1H),6.91-6.89(m,1H),4.16-4.14(m,2H),1.41-1.38(m,3H)。ES-LCMS m/z 158([M+H]+)。
參考文獻(xiàn):
[1] Patent: WO2016/37578, 2016, A1. Location in patent: Page/Page column 71; 72
[2] Patent: WO2016/38519, 2016, A1. Location in patent: Page/Page column 34; 35
[3] Patent: WO2016/38552, 2016, A1. Location in patent: Page/Page column 49
[4] Patent: WO2014/141187, 2014, A1. Location in patent: Page/Page column 112; 52; 53
[5] ACS Medicinal Chemistry Letters, 2018, vol. 9, # 7, p. 623 - 628