1314777-15-5
139022-25-6
步骤2. 将咪唑并[1,2-a]吡啶-6-羧酸盐酸盐(170 g)溶于水(600 mL)中,加热至完全溶解形成澄清溶液。随后,缓慢加入2 M NaOH水溶液,调节pH至5-6。将反应混合物置于冰水浴中冷却至0℃。通过真空过滤收集析出的沉淀,用乙醇洗涤,并在真空下干燥,得到目标产物咪唑并[1,2-a]吡啶-6-甲酸(107.2 g,收率77%),为浅黄色粉末。产物结构经1H NMR(400 MHz, DMSO-d6)和质谱(ESI+)确认:1H NMR δ 13.76-12.82(br, 1H), 9.28(s, 1H), 8.10(s, 1H), 7.68(s, 1H), 7.64-7.56(m, 2H); MS (ESI+) m/z: 163 [M + H]+。
参考文献:
[1] Patent: WO2013/127266, 2013, A1. Location in patent: Page/Page column 130
[2] Patent: WO2013/127267, 2013, A1. Location in patent: Page/Page column 81; 82
[3] Patent: WO2013/127268, 2013, A1. Location in patent: Page/Page column 59; 60
[4] Patent: WO2013/130943, 2013, A1. Location in patent: Paragraph 0181