化学合成。
化学合成
合成路线 1(1. 合成:184357-44-6)
产率:100%
合成条件:at 20℃; for 16 h;
实验步骤:步骤1:(3-羟基-2,2-二甲基丙基)氨基甲酸叔丁酯的合成得到3-氨基-2,2-二甲基-1-丙醇(1.50g,14.5mmol)的CH 2 Cl 2(70ml)溶液 加入二碳酸二叔丁酯(3.49g,16.0mmol)。 将混合物在室温下搅拌16小时。 加入饱和NH 4 Cl溶液并将混合物搅拌10分钟。 分离各层,有机相用饱和NaHCO 3溶液洗涤,干燥(Na 2 SO 4),真空浓缩,得到标题化合物,为白色固体(3.40g,定量)。 LCMS:226.20(M + Na +)。
参考文献:
- [1] Patent: WO2011/71725, 2011, A1. Location in patent: Page/Page column 53 [2] ChemMedChem, 2014, vol. 9, # 1, p. 197 - 206 [3] Patent: WO2006/57868, 2006, A1. Location in patent: Page/Page column 72 [4] Patent: WO2018/109648, 2018, A1. Location in patent: Page/Page column 52; 56 [5] Patent: US2005/54701, 2005, A1 [6] Patent: EP1548024, 2005, A1. Location in patent: Page/Page column 89-90 [7] Patent: EP2261213, 2010, A1. Location in patent: Page/Page column 43-44 [8] Patent: WO2011/71716, 2011, A1. Location in patent: Page/Page column 71 [9] Patent: WO2013/4984, 2013, A1. Location in patent: Page/Page column 67 [10] Patent: EP2746265, 2014, A1. Location in patent: Paragraph 0097 [11] Patent: EP2746265, 2015, B1. Location in patent: Paragraph 0097 [12] Patent: EP2746265, 2015, B1. Location in patent: Paragraph 0096 [13] Patent: WO2016/172496, 2016, A1. Location in patent: Paragraph 00797-00798 [14] Patent: JP2017/1991, 2017, A. Location in patent: Paragraph 0206 - 0208