化学合成。
医药; 化工
合成路线 1(1. 合成:1000342-11-9)
产率:99.1%
合成条件:With iron; ammonium chloride In ethanol; water at 90℃; for 1 h;
实验步骤:步骤4:3-氨基-5-溴-2-甲基苯甲酸甲酯[5-] 5-溴-2-甲基-3-硝基苯甲酸甲酯(17g,62.0mmol)在乙醇(85mL)中的混合物具有 加入NH 4 Cl溶液(17g,在85mL水中,317.8mmol),然后加入Fe粉末(27.8g,498.1mmol)。 将所得反应混合物在90℃下搅拌1小时。 完成后,过滤反应混合物,浓缩滤液至干。 将所得固体溶于饱和的。 碳酸氢钠溶液,用乙酸乙酯萃取。 将合并的有机层用硫酸钠干燥并浓缩,得到固体3-氨基-5-溴-2-甲基苯甲酸甲酯(15g,99.1%)。
参考文献:
- [1] Patent: WO2012/118812, 2012, A2. Location in patent: Page/Page column 312 [2] Patent: WO2012/142513, 2012, A1. Location in patent: Page/Page column 268 [3] Patent: US2014/107122, 2014, A1. Location in patent: Paragraph 0161; 0162 [4] Patent: CN105037360, 2016, B. Location in patent: Paragraph 0205; 0206; 0207 [5] Patent: WO2015/104677, 2015, A1. Location in patent: Page/Page column 69 [6] Patent: WO2013/155317, 2013, A1. Location in patent: Page/Page column 45 [7] Patent: WO2013/155464, 2013, A1. Location in patent: Paragraph 0237; 0328 [8] Patent: WO2015/57859, 2015, A1. Location in patent: Paragraph 086 [9] Patent: US2017/8904, 2017, A1. Location in patent: Paragraph 0422; 0425 [10] Patent: US2018/177750, 2018, A1. Location in patent: Paragraph 1240-1244 [11] Patent: US2012/264734, 2012, A1. Location in patent: Page/Page column 101 [12] Patent: WO2015/110999, 2015, A1. Location in patent: Page/Page column 64; 65