化学合成。
化学合成
合成路线 1（1. 合成：4167-77-5）
产率：84%
合成条件：With tetrabutyl ammonium fluoride; potassium carbonate In N,N-dimethyl-formamide at 20℃; Inert atmosphere
实验步骤：在室温下，向1,4-二溴丁烷，丙二酸二乙酯在DMF中的溶液中加入。 在N 2下加入K 2 CO 3和TBAF。 然后将反应混合物在室温下搅拌。 过夜。 然后将反应混合物用冷水（（200mL）淬灭并用10％EtOAc /己烷（3×150mL）萃取。合并的有机层用半饱和盐水（150mL×2）洗涤，然后用盐水（150mL）洗涤。 用Na 2 SO 4干燥并过滤，将滤液浓缩至干，通过快速硅胶柱纯化残余物，用2％EtOAc /己烷洗脱，得到36.7g（84％收率）无色油状物。
参考文献：
- [1] Tetrahedron Letters, 2005, vol. 46, # 4, p. 635 - 638 [2] Patent: WO2013/185202, 2013, A1. Location in patent: Paragraph 00280; 00281 [3] Patent: WO2015/95227, 2015, A2. Location in patent: Page/Page column 96; 97 [4] Journal of Medicinal Chemistry, 2018, vol. 61, # 3, p. 989 - 1000 [5] Journal of the American Chemical Society, 2010, vol. 132, # 41, p. 14409 - 14411 [6] Journal of Organic Chemistry USSR (English Translation), 1983, vol. 19, p. 474 - 480 [7] Zhurnal Organicheskoi Khimii, 1983, vol. 19, # 3, p. 541 - 548 [8] Journal of Fluorine Chemistry, 2000, vol. 102, # 1-2, p. 141 - 146 [9] Journal of Organic Chemistry, 1993, vol. 58, # 27, p. 7709 - 7717 [10] Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 1990, vol. 39, # 11, p. 2399 - 2401 [11] Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1990, # 11, p. 2646 - 2648 [12] Bulletin of the Chemical Society of Japan, 1989, vol. 62, # 10, p. 3187 - 3194 [13] Patent: US5453423, 1995, A [14] Patent: US4792563, 1988, A [15] Patent: EP2103592, 2009, A2. Location in patent: Page/Page column 41-42 [16] Organic Process Research and Development, 2014, vol. 18, # 1, p. 26 - 35 [17] Organic and Biomolecular Chemistry, 2017, vol. 15, # 12, p. 2647 - 2654 [18] New Journal of Chemistry, 2017, vol. 41, # 15, p. 6991 - 6994
