化学合成。
医药; 有机合成
合成路线 1(1. 合成:132521-66-5)
产率:68%
合成条件:With triethylamine; trichlorophosphate In toluene at 120℃; for 3 h;
实验步骤:化合物2-3的制备向2L(10g,48.5mmol)的POCl 3(80mL)溶液中加入Et 3 N(4.85g,48.5mmol)。 将溶液加热至120℃并搅拌3小时,然后真空除去溶剂。 将残余物倒入冰水中,并用DCM萃取。 将有机相用NaHCO 3和盐水洗涤,并经无水Na 2 SO 4干燥并过滤。 浓缩滤液,得到所需产物(30g,68%)。
参考文献:
- [1] Medicinal Chemistry Research, 2014, vol. 23, # 6, p. 2964 - 2975 [2] Journal of Medicinal Chemistry, 2010, vol. 53, # 11, p. 4450 - 4465 [3] Patent: WO2013/67597, 2013, A1. Location in patent: Page/Page column 78 [4] Patent: WO2018/191746, 2018, A1. Location in patent: Paragraph 0391 [5] ACS Medicinal Chemistry Letters, 2014, vol. 5, # 8, p. 921 - 926 [6] Patent: US2012/289497, 2012, A1. Location in patent: Page/Page column 42-43 [7] Patent: EP2524917, 2012, A1. Location in patent: Page/Page column 46-47 [8] Patent: WO2013/52550, 2013, A2. Location in patent: Paragraph 0221 [9] Patent: US9873694, 2018, B2. Location in patent: Page/Page column 86; 87 [10] Bioorganic and Medicinal Chemistry, 2016, vol. 24, # 11, p. 2549 - 2558 [11] Bioorganic and Medicinal Chemistry, 2003, vol. 11, # 12, p. 2541 - 2550 [12] Patent: WO2007/109810, 2007, A2. Location in patent: Page/Page column 110-111 [13] Patent: WO2013/166110, 2013, A1. Location in patent: Sheet 8 [14] Patent: WO2014/120995, 2014, A2. Location in patent: Page/Page column 178 [15] Patent: WO2016/55812, 2016, A1. Location in patent: Page/Page column 48 [16] RSC Advances, 2016, vol. 6, # 81, p. 77717 - 77734