化学合成。
化学合成
合成路线 1(1. 合成:17329-31-6)
产率:100%
合成条件:With hydrogen In methanol at 20℃; for 4 h;
实验步骤:中间体5在1L烧瓶中加入中间体5A(1g,5.23mmol)的MeOH(500ml)溶液,得到黄色悬浮液。 加入10%Pd / C(0.056g,0.523mmol)。 将混合物在室温下搅拌。 在氢气球下放置4小时。 过滤反应混合物并浓缩成黄色固体0.84g(100%)。 1H NMR(500MHz,DMSO-d6)δppm5.60(s,2H)7.05(dd,J = 8.80,2.75Hz,1H)7.16(d,J = 2.75Hz,1H)7.36(d,J = 8.80Hz,1H)7.74(s,1H)11.80(s,1H)。
参考文献:
- [1] Patent: WO2008/79759, 2008, A1. Location in patent: Page/Page column 90 [2] Patent: WO2008/79836, 2008, A2. Location in patent: Page/Page column 86 [3] Tetrahedron Letters, 2003, vol. 44, # 24, p. 4455 - 4458 [4] European Journal of Medicinal Chemistry, 2012, vol. 50, p. 264 - 273 [5] Chemical and Pharmaceutical Bulletin, 2014, vol. 62, # 12, p. 1166 - 1172 [6] Yakugaku Zasshi, 1942, vol. 62, p. 66,68; dtsch. Ref. S. 24 [7] Chem.Abstr., 1951, p. 1580 [8] Yakugaku Zasshi, 1942, vol. 62, p. 66,68; dtsch. Ref. S. 24 [9] Chem.Abstr., 1951, p. 1580 [10] Journal of Organic Chemistry, 1952, vol. 17, p. 149,153 [11] Patent: WO2006/12374, 2006, A1. Location in patent: Page/Page column 181 [12] Patent: US6339099, 2002, B1. Location in patent: Page column 43, 44 [13] Patent: US2003/225106, 2003, A1. Location in patent: Page 86 [14] Bioorganic and Medicinal Chemistry Letters, 2010, vol. 20, # 11, p. 3235 - 3239