化学合成。
化学合成
合成路线 1(1. 合成:874-37-3)
产率:90.3%
合成条件:Stage #1: With ammonium chloride In ethanol; water at 90℃; for 0.50 h; Stage #2: With iron In ethanol; water for 3 h; Reflux
实验步骤:将化合物16(2g,11.04mmol)和NH 4 Cl(2.34g,44.20mmol)的乙醇和水(2:1,3mL)溶液置于90℃油浴中并回流30分钟,然后加入铁粉 加入(2.47g,44.20mmol)。将反应物在回流下进一步搅拌3小时,并在完全监测反应后,将混合物用热水过滤并将残余物用乙醇洗涤。将滤液用饱和溶液中和。 用无水硫酸钠干燥,浓缩,得到化合物17(1.5g,收率:90.3%),用NaHCO3萃取,用乙酸乙酯萃取。
参考文献:
- [1] Patent: CN108341791, 2018, A. Location in patent: Paragraph 0142; 0143; 0145 [2] Patent: US6420567, 2002, B1 [3] Zhurnal Obshchei Khimii, 1955, vol. 25, p. 199,209; engl. Ausg. S. 183, 190 [4] Zhurnal Obshchei Khimii, 1954, vol. 24, p. 133,134; engl. Ausg. S. 131 [5] Zhurnal Obshchei Khimii, 1958, vol. 28, p. 20,25; engl. Ausg. S. 20, 24 [6] Pharmaceutical Chemistry Journal, 1990, vol. 23, # 4, p. 355 - 359 [7] Advanced Synthesis and Catalysis, 2005, vol. 347, # 2-3, p. 217 - 219 [8] Chemistry of Heterocyclic Compounds (New York, NY, United States), 1987, vol. 23, # 12, p. 1356 - 1359 [9] Khimiya Geterotsiklicheskikh Soedinenii, 1987, # 12, p. 1683 - 1687 [10] Patent: US2003/60453, 2003, A1