化学合成
化学合成
路线1:4-氨基烟醛合成(CAS:42373-30-8)
- 产率:87%
- 合成条件:Stage #1: Heating / reflux;Stage #2: With potassium carbonate In hexane
- 实验步骤:实施例25C 4-氨基烟醛将实施例25B(870mg,4.2mmol)在3N HCl(aq.)(10mL)中的溶液加热至回流过夜,并用乙醚萃取三次。用固体K₂CO₃将水层调节至pH>7,并用20%异丙醇/氯仿萃取六次。将合并的萃取液干燥(Na₂SO₄),过滤并浓缩,得到所需产物(450mg; 87%)
- 参考文献:
[1] Patent: US2003/187026, 2003, A1
[2] Patent: US2003/199511, 2003, A1. Location in patent: Page/Page column 24
[3] Journal of Organic Chemistry, 1983, vol. 48, # 20, p. 3401 - 3408
[4] Synthesis, 1999, # 6, p. 959 - 964
[5] Patent: WO2013/13817, 2013, A1. Location in patent: Page/Page column 144
[6] Patent: US2013/29961, 2013, A1. Location in patent: Paragraph 0817