化学合成。
化学合成
合成路线 1(1. 合成:4897-68-1)
产率:100%
合成条件:at 20℃; for 24.08 h;
实验步骤:i)在5分钟内将1-溴-2-碘-4-甲氧基 - 苯溴(2.8mL,54.49mmol)滴加到3-碘苯甲醚(10.01g,42.77mmol)在冰醋酸(65mL)中的溶液中)。 将得到的橙色溶液在室温下搅拌24小时。 将反应混合物用水稀释并用己烷萃取。 合并的萃取液用硫代硫酸钠水溶液(5%)和盐水洗涤,用硫酸镁干燥并减压浓缩,得到13.51g(定量收率)标题化合物。 1H NMR(400MHz,CDCl3)δppm7.47(d,1H)7.39(d,1H)6.77(dd,1H)3.77(s,3H)。
参考文献:
- [1] Patent: WO2010/132016, 2010, A1. Location in patent: Page/Page column 127-128 [2] Chemistry - A European Journal, 2006, vol. 12, # 28, p. 7398 - 7410 [3] Organic Letters, 2011, vol. 13, # 10, p. 2614 - 2617 [4] Journal of Materials Chemistry C, 2016, vol. 4, # 25, p. 5981 - 5987 [5] Angewandte Chemie - International Edition, 2007, vol. 46, # 25, p. 4744 - 4747 [6] Journal of the American Chemical Society, 2001, vol. 123, # 49, p. 12202 - 12206 [7] Journal of the American Chemical Society, 2000, vol. 122, # 51, p. 12907 - 12908 [8] European Journal of Organic Chemistry, 2015, vol. 2015, # 4, p. 786 - 801 [9] Chemistry - A European Journal, 2014, vol. 21, # 10, p. 4065 - 4070 [10] Tetrahedron, 2018, vol. 74, # 20, p. 2493 - 2499 [11] European Journal of Organic Chemistry, 2018, vol. 2018, # 38, p. 5312 - 5322 [12] Patent: US9751852, 2017, B1. Location in patent: Page/Page column 9; 10 [13] Angewandte Chemie - International Edition, 2008, vol. 47, # 42, p. 8108 - 8111 [14] Chemical Communications, 2017, vol. 53, # 44, p. 5970 - 5973 [15] Angewandte Chemie - International Edition, 2008, vol. 47, # 5, p. 888 - 890 [16] Patent: US2008/234314, 2008, A1. Location in patent: Page/Page column 41 [17] Organic Letters, 2001, vol. 3, # 5, p. 651 - 653 [18] Tetrahedron, 2010, vol. 66, # 1, p. 297 - 303 [19] Tetrahedron Letters, 2012, vol. 53, # 30, p. 3861 - 3864