2-溴-1-(3-(三氟甲基)苯基)乙酮是一种含三氟甲氧基化合物,具有较高的膜渗透性、抗代谢稳定性及与脂膜的亲和力、热稳定性和化学稳定性等特点,被广泛应用于医药化工行业。制备:往装有尾气吸收装置、回流冷凝管、温度计的100 mL三颈烧瓶中依次加入1-(3-(三氟甲基)苯基)乙酮、溴酸钠、溴化钠和四氯化碳,搅拌、加热至回流,缓慢滴加1/2体积的硫酸(60 mmol浓硫酸用2 mL水稀释所得),用气相色谱跟踪,底物完全参与反应后(约1 h),快速加入1/3体积的引发剂溶液(1.1 g偶氮二异庚腈,用7 mL四氯化碳溶解所得),体系出现剧烈回流后,继续缓慢滴加剩余的引发剂溶液和硫酸(约4.5 h内加完),继续反应至产物不再形成或副产物明显增加时(约1.5 h),降至室温、过滤,有机相用10 mL 5%的碳酸氢钠溶液洗涤、分液,有机相用无水硫酸钠干燥、浓缩,得到粗产品,经柱层析纯化(乙酸乙酯:石油醚=1:20)的洗脱液洗脱,浓缩,得到2-溴-1-(3-(三氟甲基)苯基)乙酮。
医药化工
合成路线 1(2003-10-3)
- 步骤:在冰冷却下,向市售的3'-三氟甲基苯乙酮(79.6g,0.423mol)的甲苯溶液(423mL)中加入过溴化吡啶鎓(135.4g,0.423mol);搅拌5小时,同时加热至室温;将反应液再次用冰冷却,然后滴加400mL蒸馏水以停止反应和分馏;用400mL饱和碳酸氢钠水溶液洗涤甲苯层,然后用无水硫酸镁干燥,减压浓缩,减压蒸馏,得到目标化合物。
- 条件:With pyridinium perbromide hydrobromide In toluene at 0 - 20℃; for 5 h;
- 收率:81.7%
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