化学合成。
医药; 农药
合成路线 1(1. 合成:10201-73-7)
产率:79%
合成条件:at 145℃; for 6 h; Sealed tube
实验步骤:将4-氯吡啶-2-胺(10g,78.1mmol)的甲醇钠溶液(50mL,1M溶液)在密封管中的溶液在145℃下加热6小时。 将溶剂真空浓缩,得到残余物,将其通过硅胶色谱法纯化,用10%甲醇的DCM溶液洗脱,得到7.7g,79%收率的标题化合物,为灰白色固体。 MS(ESj:m / z = 125.04 [M + H],281.75 [M / 2 + H] LCMS:t R = 0.17mm。
参考文献:
- [1] Patent: WO2015/106292, 2015, A1. Location in patent: Paragraph 00592; 00603; 00604 [2] Journal of Organometallic Chemistry, 1996, vol. 523, # 2, p. 145 - 151 [3] Australian Journal of Chemistry, 1982, vol. 35, # 9, p. 1841 - 1849 [4] Australian Journal of Chemistry, 1982, vol. 35, # 10, p. 2025 - 2034 [5] Patent: WO2012/151137, 2012, A1. Location in patent: Page/Page column 50-51 [6] Patent: WO2014/74422, 2014, A1. Location in patent: Paragraph 00165