化学合成。
医药
合成路线 1(1. 合成:1124382-72-4)
产率:96%
合成条件:With hydroxylamine hydrochloride; N-ethyl-N,N-diisopropylamine In methanol; ethanol at 20℃; for 6 h;
实验步骤:对溶胶。 向中间体50(55g,181mmol)的EtOH(300mL)溶液中加入MeOH(300mL),盐酸羟胺(62.83g,904mmol)和DIPEA(694mL,543mmol)。 上午 在r.t.搅拌 6小时 将混合物真空浓缩,将残余物悬浮在DIPE中。 滤出沉淀物。 产量:37g中间体51(产率96%)。
参考文献:
- [1] Patent: WO2013/10904, 2013, A1. Location in patent: Page/Page column 76 [2] Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 17, p. 4794 - 4800 [3] Patent: KR2015/77599, 2015, A. Location in patent: Paragraph 0096; 0099-0101 [4] Patent: KR101601354, 2016, B1. Location in patent: Paragraph 0110 - 0112 [5] Patent: US2011/190269, 2011, A1. Location in patent: Page/Page column 66 [6] Patent: WO2011/92272, 2011, A1. Location in patent: Page/Page column 139; 140 [7] Patent: US2011/201605, 2011, A1. Location in patent: Page/Page column 51 [8] Patent: US2012/225884, 2012, A1. Location in patent: Page/Page column 17 [9] Bioorganic and Medicinal Chemistry, 2018, vol. 26, # 12, p. 3227 - 3241 [10] Patent: WO2010/141796, 2010, A2. Location in patent: Page/Page column 133 [11] Patent: WO2009/155551, 2009, A1. Location in patent: Page/Page column 86 [12] Patent: WO2010/10186, 2010, A1. Location in patent: Page/Page column 52-53 [13] Patent: WO2011/101304, 2011, A2. Location in patent: Page/Page column 105 [14] Patent: WO2012/116965, 2012, A1. Location in patent: Page/Page column 34 [15] Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 17, p. 5014 - 5021 [16] Organic Process Research and Development, 2016, vol. 20, # 12, p. 2085 - 2091 [17] Patent: EP2648728, 2016, B1. Location in patent: Paragraph 0047