生產(chǎn)方法
步驟4 1-(6-氨基吡啶-3-基)乙酮的合成:在1L高壓釜中加入1-(6-氯吡啶-3-基)乙酮(40g,257.10mmol)的飽和氨水溶液(750mL)。將反應(yīng)混合物在130℃下攪拌反應(yīng)10小時。反應(yīng)完成后,冷卻混合物,并在減壓條件下濃縮。殘余物通過硅膠柱色譜法(洗脫劑比例為50:1的二氯甲烷/甲醇)進行純化,得到目標化合物1-(6-氨基吡啶-3-基)乙酮,產(chǎn)量33g,收率89%,為黃色固體。
參考文獻:
[1] Bioorganic and Medicinal Chemistry Letters, 2008, vol. 18, # 23, p. 6093 - 6096
[2] Bioorganic and Medicinal Chemistry Letters, 2008, vol. 18, # 24, p. 6482 - 6485
[3] Patent: US2007/27184, 2007, A1. Location in patent: Page/Page column 17; 19
[4] Patent: WO2017/184547, 2017, A1. Location in patent: Paragraph 00379
[5] Patent: US2007/99930, 2007, A1. Location in patent: Page/Page column 45