5349-24-6 N-丁基-2-氯乙酰胺

危险等级:IRRITANT 海关编码:2924297099

作为医药中间体，用于相关药物分子的合成研究。

医药研究

合成路线 1（1. 合成：5349-24-6）

产率：92% 合成条件：With sodium hydroxide In dichloromethane; water at 20℃; for 2 h; Cooling with ice 实验步骤：将氯乙酰氯（0.2mol，15.9mL）（CAS：79-04-9）在冰浴中缓慢滴加至中等摩尔量的正丁胺（0.2mol，14.83g）的二氯甲烷（50mL）和20％（加入完成后，加入NaOH水溶液作为溶剂，升温至室温，继续搅拌2小时。收集有机相，将5％（质量百分比）的HCl和5％（质量百分比）的NaHCO 3洗涤（3×25mL）有机相干燥并过滤，减压除去溶剂，得到中间体氯乙酰基 - 正丁胺（收率92％）。将中间产物（0.05mol，9.00g）和5,6,7,8-四氢吡啶并[1,2-α]咪唑（0.05mol，6.11g）（CAS：34167-66-3）在乙腈（50mL）中混合加入反应物，回流18H，与乙腈反应，乙酸乙酯操作重结晶，收集产物[4C-imCH 2 CONHBu] Cl（产率89％），阴离子交换树脂得到[4C-imCH 2] CONHBu] OH。 参考文献：

• [1] Patent: CN104326949, 2016, B. Location in patent: Paragraph 0060; 0061; 0063 [2] Patent: WO2007/9083, 2007, A2. Location in patent: Page/Page column 68 [3] ACS Medicinal Chemistry Letters, 2017, vol. 8, # 6, p. 678 - 681 [4] ChemMedChem, 2018, [5] Organic Letters, 2004, vol. 6, # 26, p. 4805 - 4808 [6] Journal of Medicinal Chemistry, 2014, vol. 57, # 18, p. 7590 - 7599 [7] Journal of the American Chemical Society, 1956, vol. 78, p. 2556,2557 [8] Archiv der Pharmazie (Weinheim, Germany), 2002, vol. 335, # 1, p. 15 - 21 [9] Bioorganic and Medicinal Chemistry Letters, 2012, vol. 22, # 1, p. 204 - 206 [10] Green Chemistry, 2012, vol. 14, # 6, p. 1721 - 1727 [11] Bioorganic and Medicinal Chemistry Letters, 2014, vol. 24, # 6, p. 1479 - 1483 [12] Chemical Biology and Drug Design, 2014, vol. 84, # 6, p. 685 - 696 [13] RSC Advances, 2015, vol. 5, # 60, p. 48368 - 48381 [14] Patent: CN106167497, 2016, A. Location in patent: Paragraph 0125; 0126 [15] ACS Medicinal Chemistry Letters, 2017, vol. 8, # 5, p. 527 - 532 [16] Patent: CN106543099, 2017, A. Location in patent: Paragraph 0038 [17] Patent: CN106146414, 2016, A. Location in patent: Paragraph 0150; 0151; 0152 [18] Bulletin of the Korean Chemical Society, 2018, vol. 39, # 2, p. 146 - 155 [19] Patent: CN107556210, 2018, A. Location in patent: Paragraph 0041; 0042 [20] Molecules, 2018, vol. 23, # 5,