19967-55-6 1-溴-3-甲基丁-2-酮

海关编码:2914120000

用于有机合成。

有机合成

合成路线 1（1. 合成：19967-55-6）

产率：82% 合成条件：With sodium bicarbonate; calcium chloride; bromine In methanol; water 实验步骤：参考实施例4 2-苄氧基-N- [1-（3,5-二氯苯硫基）-3-甲基-2-氧代丁基] -N-甲基乙酰胺（20）的合成向300ml无水甲醇中加入43.1mg（0.5mol）称取3-甲基-2-丁酮，并将混合物在5℃下搅拌。在10℃下在30分钟内加入27.3ml（0.5mol）溴。在10℃下搅拌1小时后，加入150ml水，将混合物升温至室温并搅拌3小时。加入300毫升水后，混合物用500毫升乙醚萃取3次。萃取液用饱和碳酸氢钠水溶液洗涤，然后用饱和盐水洗涤，并将氯化钙加入到乙醚层中。将混合物搅拌1小时以脱水。过滤乙醚层，在低于30℃下浓缩，并在减压下蒸馏缩合物，得到67.49g的1-溴-3-甲基-2-丁酮（沸点67-75℃/ 28℃）。 mmHg，产率82％）。 1 H-NMR（CDCl 3 -TMS）δppm：1.18（d，J = 6.0Hz，6H），2.99（m，1H），4.00（s，2H） 参考文献：

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