化学合成。
化学合成
合成路线 1（1. 合成：66521-54-8）
产率：51%
合成条件：at 90℃; for 12 h;
实验步骤：将4.0g（33.0mmol，1.0当量）1-（吡啶-2-基）乙-1-酮在13.1mL（99.1mmol，3.0当量）DMF二甲基缩醛中的溶液在90℃下搅拌12小时。 H。 使混合物冷却至室温，过滤收集所得沉淀物。 将固体用2×5mL乙酸乙酯洗涤并在高真空下干燥，得到3.0g（17.0mmol，51％）的（E）-3 - （二甲基氨基）-1-（吡啶-2-基）丙酯。 2-en-1-one。
参考文献：
- [1] Molecules, 2007, vol. 12, # 8, p. 2061 - 2079 [2] European Journal of Organic Chemistry, 2012, # 32, p. 6407 - 6413,7 [3] Synthetic Communications, 1993, vol. 23, # 13, p. 1897 - 1903 [4] Organic Preparations and Procedures International, 1997, vol. 29, # 3, p. 285 - 292 [5] Journal of Chemical Research, Miniprint, 1997, # 3, p. 601 - 615 [6] Chemical Communications, 2017, vol. 53, # 91, p. 12286 - 12289 [7] Organic Letters, 2018, vol. 20, # 4, p. 1256 - 1260 [8] Journal of Heterocyclic Chemistry, 2007, vol. 44, # 2, p. 355 - 361 [9] European Journal of Organic Chemistry, 2016, vol. 2016, # 18, p. 3060 - 3064 [10] Tetrahedron Letters, 1999, vol. 40, # 26, p. 4779 - 4782 [11] Dalton Transactions, 2012, vol. 41, # 13, p. 3684 - 3694 [12] Patent: WO2018/172852, 2018, A1. Location in patent: Page/Page column 204; 206 [13] European Journal of Organic Chemistry, 2005, # 17, p. 3775 - 3780 [14] Bioorganic and Medicinal Chemistry Letters, 1997, vol. 7, # 2, p. 187 - 192 [15] Synthesis, 2001, # 1, p. 55 - 62 [16] Bioorganic and Medicinal Chemistry Letters, 2007, vol. 17, # 6, p. 1641 - 1645 [17] Patent: US5859215, 1999, A [18] Patent: US4788195, 1988, A [19] Patent: US4281000, 1981, A [20] European Journal of Inorganic Chemistry, 2013, # 24, p. 4305 - 4317 [21] Patent: CN103936792, 2017, B. Location in patent: Paragraph 0093; 0094; 0095
