化学合成。
化学合成
合成路线 1（1. 合成：52085-14-0）
产率：100%
合成条件：Stage #1: With sodium hydrogencarbonate In acetonitrile at 20℃; for 0.75 h; Inert atmosphere Stage #2: Inert atmosphere; Reflux
实验步骤：将2,4-二羟基苯甲醛（3.0g，1.0当量）溶解在乙腈（220ml）中，并在室温下用NaHCO 3（2.2当量）处理45分钟，然后加入苄基溴（1.1当量）。 将反应混合物在回流下搅拌。 然后用H 2 O（100ml）淬灭，用乙酸乙酯（3×25ml）萃取。 将合并的有机层用盐水（2×15ml）洗涤，用Na 2 SO 4干燥，过滤并在真空下除去溶剂，得到标题化合物12，为白色固体，其原样使用。
参考文献：
- [1] Bioorganic and Medicinal Chemistry, 2013, vol. 21, # 15, p. 4502 - 4510 [2] Synlett, 2011, # 11, p. 1605 - 1607 [3] Organic Process Research and Development, 2011, vol. 15, # 5, p. 1149 - 1162 [4] Tetrahedron Letters, 2013, vol. 54, # 31, p. 4121 - 4124 [5] Organic Letters, 2008, vol. 10, # 21, p. 5007 - 5010 [6] Patent: US2011/144195, 2011, A1. Location in patent: Page/Page column 2; 4; 11 [7] Phosphorus, Sulfur and Silicon and the Related Elements, 2018, vol. 193, # 5, p. 306 - 316 [8] Phosphorus, Sulfur and Silicon and the Related Elements, 2018, vol. 193, # 9, p. 574 - 581 [9] Journal of Medicinal Chemistry, 2012, vol. 55, # 12, p. 5797 - 5812 [10] Bioorganic and Medicinal Chemistry Letters, 2014, vol. 24, # 15, p. 3633 - 3637 [11] European Journal of Medicinal Chemistry, 2018, vol. 143, p. 1428 - 1435 [12] Patent: WO2015/200514, 2015, A2. Location in patent: Page/Page column 69 [13] Journal of Heterocyclic Chemistry, 1987, vol. 24, # 1, p. 75 - 77 [14] Patent: WO2013/119985, 2013, A1. Location in patent: Paragraph 00335; 00336 [15] Patent: WO2018/83171, 2018, A1. Location in patent: Page/Page column 48; 49 [16] Journal of the American Chemical Society, 2010, vol. 132, # 26, p. 8828 - 8830 [17] Patent: WO2011/94560, 2011, A1. Location in patent: Page/Page column 54 [18] Patent: US9075014, 2015, B2. Location in patent: Page/Page column 39 [19] Patent: WO2012/11125, 2012, A1. Location in patent: Page/Page column 145-146 [20] Rikagaku Kenkyusho Iho, 1940, vol. 19, p. 802,803 [21] Chem.Abstr., 1940, p. 5842 [22] Bioorganic and Medicinal Chemistry Letters, 1997, vol. 7, # 11, p. 1421 - 1426 [23] Patent: US6610687, 2003, B1 [24] Tetrahedron Asymmetry, 2008, vol. 19, # 3, p. 343 - 347 [25] Bioorganic and Medicinal Chemistry Letters, 2008, vol. 18, # 19, p. 5252 - 5254 [26] Journal of Natural Products, 2009, vol. 72, # 11, p. 2072 - 2075 [27] Organic Letters, 2012, vol. 14, # 17, p. 4544 - 4547 [28] Tetrahedron Letters, 2015, vol. 56, # 11, p. 1338 - 1343
