化学合成;用于制备基于钠改性沸石的铯吸附材料;以二氨基吡嗪的钠盐为原料,经三氯氧磷和硫酸混合加热、加入原料、中和萃取精馏等步骤制备2-氯-3-氨基吡嗪(收率87%)
化学合成; 铯吸附材料制备
路线1:
- 步骤:将2,3-二氯吡嗪(5.0g,33.6mmol)和28%氨水(20mL)置于管中,密封并在100℃下搅拌18小时。将反应溶液用水稀释,过滤得到固体物质。
- 条件:With ammonia In water at 100℃; for 18 h; sealed tube
- 产率:100%
- 参考文献:[1] Patent: US2012/59162, 2012, A1. Location in patent: Page/Page column 38-39 [2] Journal of Medicinal Chemistry, 2014, vol. 57, # 10, p. 4196 - 4212 [3] Bioorganic and Medicinal Chemistry Letters, 2017, vol. 27, # 15, p. 3454 - 3459 [4] Patent: US2014/364414, 2014, A1. Location in patent: Paragraph 0438-0440 [5] Patent: WO2010/69684, 2010, A1. Location in patent: Page/Page column 96 [6] Patent: WO2013/78254, 2013, A1. Location in patent: Paragraph 00347 [7] Journal of Heterocyclic Chemistry, 1990, vol. 27, # 6, p. 1639 - 1643 [8] Patent: WO2012/80229, 2012, A1. Location in patent: Page/Page column 39 [9] Patent: US2007/105864, 2007, A1. Location in patent: Page/Page column 121 [10] Patent: US2007/117804, 2007, A1. Location in patent: Page/Page column 46-47 [11] European Journal of Medicinal Chemistry, 2015, vol. 103, p. 381 - 395 [12] Patent: WO2005/34837, 2005, A2. Location in patent: Page/Page column 41 [13] Patent: WO2005/34837, 2005, A2. Location in patent: Page/Page column 41 [14] Journal of Medicinal Chemistry, 2014, vol. 57, # 9, p. 3687 - 3706 [15] Patent: EP3252059, 2017, A1. Location in patent: Paragraph 0390; 0393; 0394 [16] Patent: US2006/47126, 2006, A1. Location in patent: Page/Page column 25 [17] Patent: US2002/52375, 2002, A1 [18] Patent: US2009/239847, 2009, A1. Location in patent: Page/Page column 46 [19] Patent: WO2011/5759, 2011, A2. Location in patent: Page/Page column 69 [20] Patent: WO2016/97918, 2016, A1. Location in patent: Page/Page column 82
路线2:
- 步骤:将2,3-二氯吡嗪(35g,0.23mol)在25%氨水(200ml)中的悬浮液在PTFE衬里的压力反应器(终端压力100psi)中在100℃下加热12小时。将反应冷却至环境温度,过滤收集得到的结晶固体。将该固体用水(150ml)研磨并干燥。
- 条件:at 100℃; for 12 h; PTFE衬里的压力反应器(终端压力100psi)
- 产率:92%
- 参考文献:[1] Patent: WO2004/41826, 2004, A1. Location in patent: Page 25-26