98977-34-5 1-N-Boc-4-氧代-3-哌啶羧酸乙酯

运输信息：常温运输。危险描述：非危险化学品。

化学合成

化学合成

路线1：

• 步骤: 将1-苄基-3-乙氧基-4-哌啶酮盐酸盐（IA）的乙醇溶液和Pd/C在1臂氢化，反应完成后加入三乙胺和（Boc）₂O，搅拌后过滤除去催化剂，浓缩萃取干燥得到产物IB。
• 条件: Stage #1: With hydrogen In ethanol at 20℃; for 15 h; Stage #2: With triethylamine In ethanol at 20℃; for 16 h;
• 收率: 100%
• 参考文献: [1] Patent: WO2008/130584, 2008, A1. Location in patent: Page/Page column 131; 135 [2] Organic Process Research and Development, 2011, vol. 15, # 5, p. 1138 - 1148 [3] Bioorganic and Medicinal Chemistry Letters, 2011, vol. 21, # 13, p. 3970 - 3975 [4] Patent: WO2011/103091, 2011, A1. Location in patent: Page/Page column 93

路线2：

• 步骤: 向0-氧代哌啶-3-羧酸乙酯盐酸盐的1M Na₂CO₃和CH₂Cl₂双相混合物中加入Boc₂O，搅拌后用2M HCl处理，萃取干燥浓缩得到产物。
• 条件: With sodium carbonate In dichloromethane; water at 20℃; for 6.50 h;
• 收率: 99%
• 参考文献: [1] Bioorganic and Medicinal Chemistry, 2008, vol. 16, # 2, p. 822 - 829 [2] Journal of Medicinal Chemistry, 2013, vol. 56, # 4, p. 1693 - 1703 [3] Bioorganic and Medicinal Chemistry, 2007, vol. 15, # 16, p. 5590 - 5603 [4] Patent: WO2008/5511, 2008, A2. Location in patent: Page/Page column 101 [5] Patent: WO2008/31772, 2008, A1. Location in patent: Page/Page column 129-130 [6] Tetrahedron, 1991, vol. 50, # 2, p. 515 - 528 [7] Patent: WO2010/138430, 2010, A1. Location in patent: Page/Page column 36 [8] Patent: WO2011/22213, 2011, A1. Location in patent: Page/Page column 32-33 [9] Tetrahedron: Asymmetry, 1993, vol. 4, # 4, p. 625 - 628 [10] Tetrahedron Asymmetry, 2004, vol. 15, # 20, p. 3281 - 3287 [11] Journal of the Chemical Society - Perkin Transactions 1, 1998, # 22, p. 3673 - 3683 [12] Organic letters, 2000, vol. 2, # 25, p. 4037 - 4040 [13] Patent: US6448263, 2002, B1 [14] Patent: US5756508, 1998, A [15] Patent: WO2008/58387, 2008, A1. Location in patent: Page/Page column 13 [16] Bioorganic and Medicinal Chemistry Letters, 2014, vol. 24, # 23, p. 5478 - 5483 [17] Patent: US2015/368242, 2015, A1. Location in patent: Page/Page column 15; 16 [18] Patent: WO2008/141462, 2008, A1. Location in patent: Page/Page column 30 [19] Patent: WO2009/87, 2008, A1. Location in patent: Page/Page column 38; 32 [20] Patent: WO2009/109608, 2009, A1. Location in patent: Page/Page column 48-49

路线3：

• 步骤: 在15℃下向4-氧代哌啶-3-羧酸乙酯的DCM溶液中滴加Et₃N，搅拌后加入（BOC）₂O，保持温度，室温搅拌过夜，浓缩后用己烷处理过滤洗涤得到产物。
• 条件: With triethylamine In dichloromethane at 10 - 20℃;
• 收率: 95.4%
• 参考文献: [1] Tetrahedron Letters, 1999, vol. 40, # 2, p. 367 - 370 [2] Patent: US9255096, 2016, B1. Location in patent: Page/Page column 47 [3] Patent: WO2005/66176, 2005, A1. Location in patent: Page/Page column 136-137 [4] European Journal of Organic Chemistry, 2003, # 4, p. 721 - 726 [5] Bioorganic and Medicinal Chemistry Letters, 2005, vol. 15, # 18, p. 4023 - 4028 [6] Patent: EP1214314, 2005, B1. Location in patent: Page/Page column 12 [7] Patent: WO2008/130615, 2008, A1. Location in patent: Page/Page column 46; 50 [8] Patent: EP1202987, 2003, B1. Location in patent: Page/Page column 11