64-17-5
50893-53-3
50893-36-2
在0°C冷卻條件下,向250 mL甲苯溶液中依次加入71.5 g(0.5 mmol)1-氯乙基氯甲酸酯、40 g乙醇和52.0 g三乙胺。加料完成后,保持反應體系在0°C下攪拌約2小時。隨后,將反應體系緩慢升溫至室溫,繼續(xù)反應1小時。反應完成后,過濾除去固體雜質(zhì),通過蒸餾純化得到78.5 g中間體1-氯乙基乙基碳酸酯(H-1)。
參考文獻:
[1] Synthesis, 1986, # 8, p. 627 - 632
[2] Patent: EP1437352, 2004, A1. Location in patent: Page 17
[3] Journal of Medicinal Chemistry, 2014, vol. 57, # 13, p. 5748 - 5763
[4] Patent: WO2016/207216, 2016, A1. Location in patent: Page/Page column 70
[5] Patent: CN107652239, 2018, A. Location in patent: Paragraph 0098