化学合成。
医药
合成路线 1(1. 合成:145549-76-4)
产率:89%
合成条件:With dicyclohexyl-carbodiimide In dichloromethane at 20℃;
实验步骤:向市售的3-氧代环丁烷羧酸(11.4g,100mmol)的无水DCM(100mL)溶液中加入DCC(31g,150mmol)和2g甲基丙-2-醇(8.9g,120mmol),然后 将混合物在室温下搅拌过夜。 将混合物用H 2 O水溶液淬灭,用DCM萃取,将有机层用盐水洗涤,经无水Na 2 SO 4干燥,过滤并真空浓缩。 通过柱纯化残余物,得到试剂R-28b(15.1g,89%收率)。
参考文献:
- [1] Patent: WO2014/131855, 2014, A1. Location in patent: Page/Page column 77 [2] Journal of Medicinal Chemistry, 2016, vol. 59, # 19, p. 8967 - 9004 [3] Journal of Organic Chemistry, 1993, vol. 58, # 1, p. 100 - 110 [4] Journal of Medicinal Chemistry, 2017, vol. 60, # 2, p. 627 - 640 [5] Patent: US2009/298894, 2009, A1. Location in patent: Page/Page column 44 [6] Patent: US2017/283406, 2017, A1. Location in patent: Paragraph 0685; 0686