化学合成。
化学合成
合成路线 1(1. 合成:74316-55-5)
产率:71%
合成条件:at 20℃; for 5 h;
实验步骤:步骤1:5-溴-8-甲基喹啉将8-甲基喹啉在H 2 SO 4(浓)中的溶液(0.3M)用Ag 2 SO 4(1.5当量)处理,并加入溴(1.0当量)。 将反应混合物在室温下搅拌5小时,然后倒入冰中。 过滤沉淀物并丢弃。 剩余的溶液用Na 2 CO 3水溶液(饱和溶液)碱化,水相用EtOAc萃取。 将合并的有机层干燥并蒸发,得到(71%)标题化合物,为固体; MS(ES +)m / z 222,224(M + H)+。
参考文献:
- [1] Chemistry of Heterocyclic Compounds (New York, NY, United States), 1980, vol. 16, # 3, p. 275 - 277 [2] Khimiya Geterotsiklicheskikh Soedinenii, 1980, vol. 16, # 3, p. 366 - 368 [3] Tetrahedron, 2005, vol. 61, # 41, p. 9696 - 9704 [4] Bioorganic and Medicinal Chemistry, 2010, vol. 18, # 8, p. 2836 - 2848 [5] Patent: WO2007/28789, 2007, A1. Location in patent: Page/Page column 34 [6] Journal of the American Chemical Society, 2014, vol. 136, # 11, p. 4141 - 4144 [7] Chemistry of Heterocyclic Compounds (New York, NY, United States), 1988, vol. 24, # 8, p. 892 - 897 [8] Khimiya Geterotsiklicheskikh Soedinenii, 1988, # 8, p. 1084 - 1090 [9] Patent: WO2013/96194, 2013, A1. Location in patent: Page/Page column 31-32 [10] Advanced Synthesis and Catalysis, 2017, vol. 359, # 17, p. 2912 - 2917 [11] Patent: WO2009/141386, 2009, A1. Location in patent: Page/Page column 162; 163