路线1:乙酰乙酸乙酯与1,1-二甲氧基-N,N-二甲基甲胺反应
- 步骤:将3-氧代丁酸乙酯(250ml,1961mmol)在室温下搅拌,逐滴加入1,1-二甲氧基-N,N-二甲基甲胺(327ml,2452mmol),室温搅拌过夜;真空浓缩反应混合物,与甲苯(3×300mL)共沸后高真空处理,得到油状物产物,不经纯化直接使用。
- 条件:20℃;
- 收率:100%;
- 参考文献:[1] Patent: WO2006/73361, 2006, A1. Location in patent: Page/Page column 147 [2] Patent: US2007/244088, 2007, A1. Location in patent: Page/Page column 38 [3] Patent: US2008/9523, 2008, A1. Location in patent: Page/Page column 18; 19 [4] Patent: WO2008/4943, 2008, A1. Location in patent: Page/Page column 59 [5] Patent: WO2008/4942, 2008, A1. Location in patent: Page/Page column 56 [6] Patent: WO2009/48765, 2009, A1. Location in patent: Page/Page column 13 [7] Patent: WO2008/141020, 2008, A1. Location in patent: Page/Page column 59 [8] Journal of Labelled Compounds and Radiopharmaceuticals, 2011, vol. 54, # 6, p. 324 - 331 [9] Journal of Molecular Structure, 2019, vol. 1175, p. 551 - 565 [10] RSC Advances, 2017, vol. 7, # 45, p. 28483 - 28488 [11] Journal of Heterocyclic Chemistry, 1987, vol. 24, p. 693 - 695 [12] Tetrahedron Letters, 1998, vol. 39, # 3-4, p. 213 - 216 [13] Journal of Heterocyclic Chemistry, 1987, vol. 24, # 6, p. 1669 - 1675 [14] Chemical Biology and Drug Design, 2018, vol. 92, # 3, p. 1683 - 1691 [15] Patent: US2012/22251, 2012, A1. Location in patent: Page/Page column 27 [16] Patent: EP2602260, 2013, A1. Location in patent: Paragraph 0141 [17] Patent: EP1364949, 2003, A1. Location in patent: Page/Page column 100 [18] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1992, # 20, p. 2603 - 2608 [19] Synthesis, 1990, # 1, p. 70 - 72 [20] Journal of Heterocyclic Chemistry, 1997, vol. 34, # 1, p. 177 - 193 [21] Patent: US5321002, 1994, A [22] Patent: WO2007/8140, 2007, A1. Location in patent: Page/Page column 86 [23] Patent: US2008/176827, 2008, A1. Location in patent: Page/Page column 18 [24] Patent: WO2008/85119, 2008, A1. Location in patent: Page/Page column 103 [25] Patent: US2004/147561, 2004, A1. Location in patent: Page 45 [26] Patent: US2005/20564, 2005, A1. Location in patent: Page/Page column 14 [27] Patent: WO2010/5385, 2010, A1. Location in patent: Page/Page column 77; 85 [28] Bioorganic and Medicinal Chemistry Letters, 2009, vol. 19, # 23, p. 6591 - 6594 [29] Patent: US2006/211603, 2006, A1. Location in patent: Page/Page column 80-81 [30] Patent: WO2011/42797, 2011, A1. Location in patent: Page/Page column 69 [31] Bioorganic and Medicinal Chemistry Letters, 2012, vol. 22, # 21, p. 6756 - 6761 [32] Organic Process Research and Development, 2012, vol. 16, # 11, p. 1846 - 1853 [33] Organic Process Research and Development, 2012, vol. 16, # 10, p. 1618 - 1625 [34] Organic Process Research and Development, 2013, vol. 17, # 12, p. 1543 - 1551 [35] Research on Chemical Intermediates, 2016, vol. 42, # 3, p. 2597 - 2617 [36] Monatshefte fur Chemie, 2016, vol. 147, # 7, p. 1257 - 1276 [37] Patent: WO2017/176812, 2017, A1. Location in patent: Paragraph 0271 [38] Patent: US2004/220170, 2004, A1. Location in patent: Page 16