51012-64-7 2-溴-1-(3-甲基苯基)乙基-1-酮

运输信息：冰袋运输。危险描述：非危险化学品。

化学合成

化学合成

合成路线 1（1. 合成：51012-64-7）

• 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。
• 条件：at 40℃; for 6 h; Green chemistry
• 产率：94%
• 参考文献：[1] European Journal of Organic Chemistry, 2016, vol. 2016, # 1, p. 116 - 121 [2] Tetrahedron Letters, 2014, vol. 55, # 7, p. 1373 - 1375 [3] Journal of Organic Chemistry, 2013, vol. 78, # 18, p. 9190 - 9195 [4] Tetrahedron Letters, 2016, vol. 57, # 45, p. 4983 - 4986 [5] Tetrahedron, 2016, vol. 72, # 27-28, p. 3818 - 3822 [6] Chinese Journal of Chemistry, 2016, vol. 34, # 12, p. 1251 - 1254

合成路线 2（2. 合成：51012-64-7）

• 步骤：将Oxone（1.352g，2.2mmol）加入到充分搅拌的底物（2mmol）和NH₄Br（0.215g，2.2mmol）的甲醇（10ml）溶液中，并将反应混合物在室温下搅拌（或回流温度）。在反应完成后，通过TLC监测，将反应混合物用硫代硫酸钠水溶液淬灭，并用乙酸乙酯（3.x.25ml）萃取。最后，将合并的有机层用水洗涤，用无水硫酸钠干燥，过滤并真空除去溶剂，得到粗残余物，将其通过硅胶柱色谱（细于200目）进一步纯化，得到纯产物。所有产物均在1H NMR和质谱数据的基础上鉴定。
• 条件：With Oxone; ammonium bromide In methanol for 0.67 h; Reflux
• 产率：96%
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