化学合成。
化学合成; 医药
合成路线 1(1. 合成:1131-94-8)
产率:44.4%
合成条件:With copper(ll) sulfate pentahydrate; sodium hydroxide In water at 150℃; for 20 h; Sealed tube
实验步骤:向125mL密封管中加入氢氧化钠(24.5g,612mmol),硫酸铜五水合物(1.02g,4.08mmol),水(60mL)溶解,冷却,得到3-溴-4-甲氧基苯乙酸(10g,40.8mmol) ),将密封管塞住并在150℃油浴中搅拌20小时,冷却至室温,滴加浓盐酸pH 3,抽滤,滤饼用水洗涤,收集排出的滤饼并通过以下方法纯化: 柱层析(二氯甲烷:甲醇30:1),得到灰白色固体(3.3g,收率44.4%)。
参考文献:
- [1] Journal of Organic Chemistry, 1984, vol. 49, # 11, p. 2061 - 2063 [2] Synthesis, 2011, # 2, p. 217 - 222 [3] Patent: WO2010/75469, 2010, A1. Location in patent: Page/Page column 115 [4] Patent: US2011/9628, 2011, A1. Location in patent: Page/Page column 37 [5] Patent: CN105481849, 2016, A. Location in patent: Paragraph 0461; 0465; 0466 [6] Patent: CN105481850, 2016, A. Location in patent: Paragraph 0648; 0652; 0653 [7] Patent: CN105418601, 2016, A. Location in patent: Paragraph 0494; 0495