化学合成,医药中间体。
医药; 有机合成
合成路线 1(1. 合成:99-81-0)
产率:77%
合成条件:at 40℃; for 6 h; Green chemistry
实验步骤:一般步骤:将卤代炔(0.5mmol),AgF(5mol%)和水(1当量)在TFA(1mL)中的混合物在40℃下搅拌6小时,然后蒸馏出TFA以再次使用。 通过柱色谱分离残余物,得到纯样品。
参考文献:
- [1] Tetrahedron Letters, 2014, vol. 55, # 7, p. 1373 - 1375 [2] Chinese Journal of Chemistry, 2016, vol. 34, # 12, p. 1251 - 1254 [3] Tetrahedron Letters, 2016, vol. 57, # 45, p. 4983 - 4986
合成路线 2(2. 合成:99-81-0)
产率:95%
合成条件:With ferric(III) bromide; silica gel In dichloromethane at 20℃; for 0.17 h;
实验步骤:一般步骤:向5mL圆底烧瓶中加入FeCl 3(0.25mmol),硅胶(100mg)和DCM(2mL)。 然后缓慢注入含有α-重氮 - 酮(0.50mmol)的1mL二氯甲烷溶液。 在室温下搅拌10分钟后,将反应混合物真空浓缩,并通过柱色谱法用10:1 PE / EA纯化,得到所需的α-卤代酮。
参考文献:
- [1] Tetrahedron Letters, 2018, vol. 59, # 13, p. 1200 - 1203
合成路线 3(3. 合成:99-81-0)
产率:99%
合成条件:With copper(ll) bromide In ethyl acetate at 60 - 65℃; for 8 h;
实验步骤:2-1-1:α-溴-4-硝基苯乙酮的制备将5g(30.3mmol)4-硝基苯乙酮溶于150ml乙酸乙酯中,并向其中加入13.5g(60.6mmol)溴化铜(II),然后 在反应完成后,将反应液冷却至室温,滤出反应过程中形成的盐。用碳酸氢钠饱和溶液洗涤滤液三次,反应完成后,将反应液冷却至室温。 将该溶液用无水硫酸镁干燥,减压过滤,减压蒸馏,然后在约40℃下真空干燥,得到7.3g(产率:99%)所需化合物,然后直接进行后续反应。 .Mass(M +):245.1
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