化学合成。
化学合成
合成路线 1(1. 合成:754131-60-7)
产率:78%
合成条件:With N-Bromosuccinimide In tetrachloromethane for 4 h; Reflux
实验步骤:将6a(1g,5.8mmol),过氧化苯甲酰(101mg,0.4mmol)和NBS(1.1g,6.39mmol)在CCI 4(58mL)中的混合物在回流下加热4小时。 将反应混合物冷却至室温,用H 2 O淬灭并用DCM(3×30mL)萃取。 将合并的有机层用Na 2 SO 4干燥,过滤并减压浓缩。 通过硅胶CC纯化残余物,用PE:EA = 15:1洗脱,得到6b(1.1g,78%收率),为黄色油状物。
参考文献:
- [1] Patent: WO2011/107248, 2011, A1. Location in patent: Page/Page column 43 [2] Patent: EP2784077, 2014, A1. Location in patent: Paragraph 0060; 0061 [3] Patent: US2014/343089, 2014, A1. Location in patent: Paragraph 0066 [4] Patent: WO2009/51715, 2009, A1. Location in patent: Page/Page column 33 [5] Patent: WO2004/98607, 2004, A1. Location in patent: Page/Page column 51 [6] Patent: WO2011/56440, 2011, A1. Location in patent: Page/Page column 31-32