化学合成。
医药; 化工
合成路线 1（1. 合成：100125-12-0）
产率：63%
合成条件：for 12 h; Reflux
实验步骤：在500毫升瓶中，加入200毫升1-氯丁烷，1,10-O-苯酚，5克，换句话说，27.8毫摩尔，S2Cl212.3克，换句话说91.1毫摩尔，吡啶7.10克，换句话说，89.8毫摩尔，液体溴，14克，换言之87.6mmol，回流反应12h，在反应过程中产生大量固体。冷却至室温，反应液体拉出担心，用大量氢氧化钠洗涤固体，用滤液CHCl3萃取，有机相打开车床，并结合固体拉出担心，干燥CHCl3短。将CHCl3浓缩至60ml后，然后加入溴3.0g，换句话说19mmol在室温下搅拌30分钟，形成黄色的Phen-Br2络合物。拉出担心，用200-300目固体硅胶作固定相，二氯甲烷/乙酸乙酯= 1/1洗脱剂制备柱层析分离，然后用甲苯重结晶，得白色针状固体5.9g，收率63％，
参考文献：
- [1] Tetrahedron Letters, 1999, vol. 40, # 17, p. 3395 - 3396 [2] Tetrahedron, 2012, vol. 68, # 39, p. 8216 - 8221 [3] European Journal of Inorganic Chemistry, 2009, # 33, p. 4962 - 4971 [4] Canadian Journal of Chemistry, 1997, vol. 75, # 10, p. 1336 - 1339 [5] Patent: CN105294781, 2016, A. Location in patent: Paragraph 0073; 0083; 0084 [6] Tetrahedron Letters, 2004, vol. 45, # 13, p. 2801 - 2803 [7] Inorganic Chemistry Communications, 2010, vol. 13, # 12, p. 1387 - 1390 [8] ChemPlusChem, 2016, vol. 81, # 1, p. 73 - 79 [9] Journal of the American Chemical Society, 2015, vol. 137, # 7, p. 2665 - 2673 [10] RSC Advances, 2016, vol. 6, # 33, p. 27360 - 27369 [11] Tetrahedron, 2013, vol. 69, # 17, p. 3523 - 3529 [12] European Journal of Organic Chemistry, 2013, # 26, p. 5893 - 5901 [13] Journal of the American Chemical Society, 2015, vol. 137, # 26, p. 8633 - 8643 [14] Journal of Photochemistry and Photobiology A: Chemistry, 2012, vol. 241, p. 1 - 7 [15] Chemistry Letters, 1995, # 9, p. 785 - 786 [16] Molecular Crystals and Liquid Crystals Science and Technology Section A: Molecular Crystals and Liquid Crystals, 2001, vol. 370, p. 387 - 390 [17] Patent: KR2016/83184, 2016, A. Location in patent: Paragraph 0094-0097
