化学合成。
医药中间体
合成路线 1(1. 合成:100644-65-3)
产率:100%
合成条件:With triethylamine; hydrazine In tetrahydrofuran; water at 20℃; for 4 h;
实验步骤:向THF(40mL)和H 2 O(4mL)的混合物中加入2-氨基-4,6-二氯嘧啶-5-甲醛(1.92g,10mmol)和三乙胺(1.59mL,11.5mmol)的混悬液 在室温下滴加肼(64%,486μ,10mmol) 将反应混合物连续搅拌4小时,然后在真空下除去挥发性物质。 将残余物用H 2 O沉淀。 将沉淀物用H 2 O洗涤,并在真空下干燥,得到标题化合物(1.8g,定量),为黄色固体。 13CNMRδ(DMSO-de,75MHz)161.5(C-2),157.5(C-4),153.2(C-7a),132.7(C-5),105.8(C-4a)。 MS(m / z)170 [M + H] +。
参考文献:
- [1] Patent: WO2014/96423, 2014, A1. Location in patent: Page/Page column 50 [2] Patent: CN103804447, 2016, B. Location in patent: Paragraph 0076; 0082; 0083; 0084 [3] Synlett, 2011, # 13, p. 1900 - 1904 [4] Patent: WO2012/135084, 2012, A1. Location in patent: Page/Page column 17 [5] Patent: US2012/202785, 2012, A1. Location in patent: Page/Page column 262 [6] Patent: WO2012/135083, 2012, A1. Location in patent: Page/Page column 20 [7] Heterocycles, 1985, vol. 23, # 10, p. 2521 - 2524 [8] Helvetica Chimica Acta, 1986, vol. 69, # 7, p. 1602 - 1613 [9] Patent: CN108371662, 2018, A. Location in patent: Paragraph 0113; 0114; 0117; 0118 [10] Patent: US2004/220194, 2004, A1. Location in patent: Page 8 [11] Patent: US2005/239795, 2005, A1. Location in patent: Page/Page column 10 [12] Bioorganic and Medicinal Chemistry Letters, 2011, vol. 21, # 8, p. 2497 - 2501 [13] Patent: WO2011/35009, 2011, A1. Location in patent: Page/Page column 77 [14] Patent: WO2007/134828, 2007, A1. Location in patent: Page/Page column 70