化学合成。
化学合成
合成路线 1(1. 合成:4996-22-9)
产率:52%
合成条件:for 36 h; Reflux
实验步骤:通用方法:将底物(0.6mmol),溴乙烯2a(0.06mmol)的DMSO(1.1mL)混合物在敞口烧瓶中加热(油浴温度,反应时间在refPreviewPlaceHolderTable 2中规定)。 在反应完成后(通过TLC检查),将反应混合物用水(11mL)稀释,用NaCl饱和并用乙酸乙酯(5.x.4mL)萃取。 仅在合成芳基乙二醛的情况下,有机层另外用Na 2 CO 3(0.12mmol,在2mL水中),用饱和NaCl水溶液洗涤,并用无水Na 2 SO 4干燥。 萃取物的柱色谱(洗脱液:梯度石油醚/乙酸乙酯)得到纯产物。
参考文献:
- [1] Tetrahedron Asymmetry, 2010, vol. 21, # 18, p. 2244 - 2248 [2] Tetrahedron, 2011, vol. 67, # 41, p. 8000 - 8008 [3] Journal of Fluorine Chemistry, 2010, vol. 131, # 12, p. 1289 - 1296 [4] Tetrahedron Letters, 2011, vol. 52, # 31, p. 4036 - 4038 [5] Tetrahedron, 2013, vol. 69, # 1, p. 22 - 28 [6] Synlett, 2013, vol. 24, # 8, p. 998 - 1000 [7] Tetrahedron, 2017, vol. 73, # 47, p. 6587 - 6596 [8] Journal of Organometallic Chemistry, 2013, vol. 744, p. 101 - 107 [9] Journal of Sulfur Chemistry, 2013, vol. 34, # 5, p. 464 - 473 [10] Journal of the American Chemical Society, 2013, vol. 135, # 45, p. 16849 - 16852 [11] Journal of Fluorine Chemistry, 2014, vol. 168, p. 151 - 157 [12] Tetrahedron Letters, 2015, vol. 56, # 32, p. 4701 - 4703 [13] Turkish Journal of Chemistry, 2015, vol. 39, # 2, p. 244 - 254 [14] Research on Chemical Intermediates, 2015, vol. 41, # 10, p. 7263 - 7272 [15] Australian Journal of Chemistry, 2015, vol. 68, # 10, p. 1529 - 1534 [16] Journal of Organic Chemistry, 2016, vol. 81, # 15, p. 6402 - 6408 [17] Journal of the Iranian Chemical Society, 2017, vol. 14, # 11, p. 2299 - 2304 [18] Journal of Heterocyclic Chemistry, 2017, vol. 54, # 6, p. 3163 - 3168 [19] Heterocyclic Communications, 2018, vol. 24, # 1, p. 37 - 41 [20] Tetrahedron Letters, 2018, vol. 59, # 31, p. 2970 - 2974 [21] Organic and Biomolecular Chemistry, 2018, vol. 16, # 38, p. 6998 - 7003 [22] Heterocyclic Communications, 2018, vol. 24, # 6, p. 297 - 302