化学合成,AZD9291中间体2。
医药
合成路线 1(1. 合成:1421372-94-2)
产率:99%
合成条件:at 80℃; for 6 h;
实验步骤:在室温下,向2L反应烧瓶中加入1000ml 2-戊醇,50g 3-(2-氯-4-嘧啶基)-1-甲基-1H-吲哚,42g 4-氟-2 - 甲氧基-5-硝基苯胺,3.54g对甲苯磺酸,将混合物加热至80℃并反应6小时。将混合物冷却至25℃至28℃,过滤,滤饼用50℃洗涤。 将滤饼干燥后,在真空烘箱中干燥,得到80.1g黄色固体,收率:99.0%。
参考文献:
- [1] Patent: CN107188888, 2017, A. Location in patent: Paragraph 0061-0063 [2] European Journal of Medicinal Chemistry, 2017, vol. 135, p. 12 - 23 [3] Patent: WO2013/14448, 2013, A1. Location in patent: Page/Page column 138 [4] Journal of Medicinal Chemistry, 2014, vol. 57, # 20, p. 8249 - 8267 [5] Patent: CN107043369, 2017, A. Location in patent: Paragraph 0395; 0396; 0397; 0398 [6] Patent: CN107793413, 2018, A. Location in patent: Paragraph 0168; 0169; 0174; 0175 [7] Patent: CN108623567, 2018, A. Location in patent: Paragraph 0056; 0057; 0058 [8] Patent: CN106967050, 2017, A. Location in patent: Paragraph 0020; 0021 [9] Patent: CN107216313, 2017, A. Location in patent: Paragraph 0053; 0054 [10] Patent: WO2018/119441, 2018, A1. Location in patent: Paragraph 00892; 00893 [11] Patent: EP3181559, 2017, A1. Location in patent: Paragraph 0047 [12] Patent: EP3216786, 2017, A1. Location in patent: Paragraph 0102-0103 [13] Patent: WO2017/205459, 2017, A1. Location in patent: Paragraph 0154 [14] Patent: WO2017/117070, 2017, A1. Location in patent: Paragraph 00103