化学合成。
化学合成
合成路线 1(1. 合成:13726-17-5)
产率:99%
合成条件:With borane-THF In tetrahydrofuran for 2.17 h; Reflux
实验步骤:C.(4-氯-3-甲氧基苯基)甲-1-醇(0201)的合成向4-氯-3-甲氧基苯甲酸(4.88g,26.2mmol)的THF(50mL)溶液中加入硼烷 - 在10分钟内通过加料漏斗进行THF络合物(52mL 1M THF溶液,52mmol)。 将反应混合物回流2小时,冷却,用EtOAc萃取,用水,5%Na 2 CO 3和盐水洗涤,干燥并真空浓缩,得到(4-氯-3-甲氧基苯基)甲-1-醇(4.5g,99%))。 ES-MS(M + H-H 2 O)+ = 155,157(CI)。
参考文献:
- [1] Patent: US2002/77486, 2002, A1 [2] Patent: US6906063, 2005, B2 [3] Patent: EP2314593, 2016, B1. Location in patent: Paragraph 0201 [4] Journal of Medicinal Chemistry, 1987, vol. 30, # 10, p. 1887 - 1891 [5] Journal of Medicinal Chemistry, 1992, vol. 35, # 23, p. 4408 - 4414 [6] Patent: WO2010/9069, 2010, A1. Location in patent: Page/Page column 47 [7] Tetrahedron Letters, 1986, vol. 27, # 45, p. 5397 - 5400 [8] Journal of Medicinal Chemistry, 1982, vol. 25, # 4, p. 352 - 358 [9] Patent: WO2005/42516, 2005, A2. Location in patent: Page/Page column 95 [10] Russian Chemical Bulletin, 2012, vol. 61, # 8, p. 1616 - 1621 [11] Izv. Akad. Nauk, Ser. Khim., 2012, # 8, p. 1599 - 1604 [12] Patent: EP1887000, 2008, A1. Location in patent: Page/Page column 106-107