化学合成。
化学合成
合成路线 1(1. 合成:2314-37-6)
产率:85%
合成条件:With N-iodo-succinimide; bis(trifluoromethanesulfonyl)imidategold(I) In 1,2-dichloro-ethane; toluene at 85℃; for 14 h;
实验步骤:一般步骤:向搅拌的底物(1mmol)的CH 2 Cl 2或(CH 2 Cl)2(0.1M)溶液中加入Ph3PAuNTf2(0.025mmol,19mg;络合物Ph3PAuNTf2甲苯,2:1),然后加入N-碘代琥珀酰亚胺(1.1)。 mmol,248mg)。 将所得溶液在室温下搅拌。 或在回流下直至原料完全转化。 在减压下除去溶剂后,通过快速柱色谱法使用不同梯度的己烷和EtOAc纯化粗物质,得到纯的所需产物。
参考文献:
- [1] European Journal of Organic Chemistry, 2000, # 8, p. 1527 - 1533 [2] European Journal of Organic Chemistry, 2012, # 30, p. 5935 - 5942,8 [3] Synthesis, 2010, # 16, p. 2776 - 2786 [4] Organic letters, 2003, vol. 5, # 4, p. 415 - 418 [5] Tetrahedron Letters, 1997, vol. 38, # 35, p. 6305 - 6306 [6] Synlett, 2014, vol. 25, # 3, p. 399 - 402 [7] Synthetic Communications, 2007, vol. 37, # 21, p. 3855 - 3860 [8] Journal of Organic Chemistry, 2017, vol. 82, # 2, p. 1205 - 1217 [9] Organic Letters, 2018, vol. 20, # 23, p. 7726 - 7730 [10] Journal of Organic Chemistry, 2006, vol. 71, # 3, p. 1027 - 1032 [11] Bioorganic and Medicinal Chemistry Letters, 2012, vol. 22, # 21, p. 6731 - 6734 [12] Patent: WO2009/76602, 2009, A1. Location in patent: Page/Page column 124 [13] Journal of the Chemical Society, 1956, p. 1417,1418, 1421 [14] Journal fuer Praktische Chemie (Leipzig), 1899, vol. <2> 59, p. 143 [15] Tetrahedron Letters, 2004, vol. 45, # 43, p. 8083 - 8085 [16] Patent: WO2006/82245, 2006, A1. Location in patent: Page/Page column 156 [17] Patent: US2005/65066, 2005, A1. Location in patent: Page/Page column 69 [18] Patent: WO2004/80480, 2004, A1. Location in patent: Page/Page column 150 [19] Patent: WO2006/5683, 2006, A1. Location in patent: Page/Page column 151 [20] Patent: US2003/229120, 2003, A1. Location in patent: Page 52