化学合成。
化学合成
合成路线 1(1. 合成:10201-71-5)
产率:100%
合成条件:With palladium 10% on activated carbon; hydrogen In methanol; ethyl acetate for 3 h;
实验步骤:在氮气氛下,向2-硝基-3-甲氧基吡啶(32g,208mmol)的EtOAc(150mL)和MeOH(35mL)溶液中加入10%钯碳(1.5g,1.4mmol)。 将该混合物用H 2吹扫三次,并将混合物在氢气氛下搅拌3小时。 将反应混合物用N 2吹扫三次,通过硅藻土过滤,并将滤饼用EtOAc(2×35ml)洗涤。 浓缩合并的滤液,高真空干燥,得到25.8克(100%)2-氨基-3-甲氧基吡啶:LCMS(m / z):125.0(MH +); 1H NMR(300MHz,CDCl3):7.66(m,1H),6.90(m,1H),6.61(m,2H),4.64(s,br,2H),3.83(s,3H)。
参考文献:
- [1] Patent: US2013/210818, 2013, A1. Location in patent: Paragraph 0380 [2] Patent: WO2009/115572, 2009, A2. Location in patent: Page/Page column 114-115 [3] Patent: WO2014/206903, 2014, A1. Location in patent: Page/Page column 15; 16 [4] Green Chemistry, 2017, vol. 19, # 3, p. 809 - 815 [5] Patent: WO2013/92739, 2013, A1. Location in patent: Page/Page column 16 [6] Patent: WO2010/96389, 2010, A1. Location in patent: Page/Page column 45; 48 [7] Patent: WO2010/135014, 2010, A1. Location in patent: Page/Page column 53-55 [8] Patent: US2011/81316, 2011, A1. Location in patent: Page/Page column 14 [9] Patent: US2009/22670, 2009, A1. Location in patent: Page/Page column 19 [10] Journal of the American Chemical Society, 1947, vol. 69, p. 1147,1148 [11] Recueil des Travaux Chimiques des Pays-Bas, 1955, vol. 74, p. 1171,1174 [12] Australian Journal of Chemistry, 1995, vol. 48, # 5, p. 1031 - 1038 [13] Patent: WO2010/100127, 2010, A1. Location in patent: Page/Page column 71-72 [14] Patent: US9096593, 2015, B2. Location in patent: Page/Page column 114 [15] ChemCatChem, 2016, vol. 8, # 8, p. 1485 - 1489 [16] European Journal of Organic Chemistry, 2018, vol. 2018, # 2, p. 209 - 214 [17] Applied Catalysis A: General, 2018, vol. 559, p. 127 - 137