3349-64-2 3,4-二氢-1(2H)-萘酮肟

危险性质：非危险化学品

化学合成。

化学合成

合成路线 1（1. 合成：3349-64-2）

产率：95% 合成条件：With hydroxylamine hydrochloride; sodium acetate In ethanol; water 实验步骤：步骤A：1-四氢萘酮肟在室温下，在装有顶置式搅拌器，温度探针和回流冷凝器的蒸汽浴装置中的4颈50L烧瓶中加入4.6L水，加入3.72Kg（27.36mol）搅拌下加入乙酸钠，然后加入1.9Kg盐酸羟胺（27.36mol）。在室温下向该浆液中加入12L乙醇，然后加入1.994Kg（13.68mol）1-四氢萘酮。使用额外的乙醇（1.7L）冲洗漏斗并加入到反应混合物中。将得到的浅橙色浆液在40分钟内加热至75℃并在75°-85℃下再保持75分钟。借助于在烧瓶周围填充的冰冷却反应混合物。当内部温度达到32℃时，将反应混合物在15分钟内泵入200L容器中所含的60L冰中。用另外2L水洗涤反应容器，将其加入200L容器中。当冰融化时，将混合物通过滤垫过滤，并将湿滤饼用4L水洗涤。将湿滤饼抽吸干燥1小时，然后转移至两个盘中，并在40℃下真空干燥2天，得到2.094Kg（13.01mol，95％）产物。 1 H NMR（250MHz，CDCl 3）：1.90（m，2H），2.80（t，6Hz，2H），2.88（t，6Hz，2H），7.15-7.35（m，3H），7.90（d， 8 Hz，1H），8.9（br s，1H）。 参考文献：

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