化学合成。
化学合成
合成路线 1(1. 合成:2941-48-2)
产率:95%
合成条件:With sulfuryl dichloride In (2S)-N-methyl-1-phenylpropan-2-amine hydrate at 0℃; for 1.25 h;
实验步骤:将得自Aldrich的5-氯 - 苯噻唑-2-硫醇(2g,9.9mmol)缓慢加入得自Aldrich的硫酰氯(20mL)中并搅拌1小时,然后加热至50℃。 15分钟。 冷却混合物,缓慢倒入冰水中并搅拌30分钟。 产物从溶液中沉淀出来,为黄色固体,真空过滤收集,在空气流下干燥,然后高真空干燥,得到1.92g(96%)化合物250. 1H NMR(400MHz,DMSO-d6)δ8.18 (d,J = 8.7Hz,1H),8.1(d,J = 2.0,1H),7.59(dd,J = 8.7,2.1Hz,1H)。
参考文献:
- [1] Patent: US2005/250820, 2005, A1. Location in patent: Page/Page column 71 [2] Synthesis (Germany), 2018, vol. 50, # 10, p. 2027 - 2032 [3] Patent: WO2014/176258, 2014, A1. Location in patent: Page/Page column 29 [4] Patent: WO2007/146066, 2007, A2. Location in patent: Page/Page column 88 [5] Patent: WO2009/55357, 2009, A1. Location in patent: Page/Page column 35 [6] Journal of Organic Chemistry, 2009, vol. 74, # 8, p. 3229 - 3231 [7] Patent: WO2011/131975, 2011, A1. Location in patent: Page/Page column 26