这次做的二苯甲酮肟只是我的合成路线的中间体。
实验本来还有后续操作的，可惜温度没有控制好，东西没做出来。
明天重做这个合成的时候，还会再做二苯甲酮肟。下次发中文，这次就不翻译了。
实验本来还有后续操作的，可惜温度没有控制好，东西没做出来。
明天重做这个合成的时候，还会再做二苯甲酮肟。下次发中文，这次就不翻译了。
17996
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Preparation of Diphenylketone Oxime （二苯甲酮肟的制备）
Submitted by P. Carneades C from YuanHe Institute
A mixture of 5.0g of diphenylketone, 3.0g of hydroxylamine hydrochloride, 5.0g of sodium hydroxide is placed in a 150mL single-necked flask. Then cover the mixture with ethanol immediately (Note 1) and a few drops of water is added. Heat the flask on a steam bath for 10 minutes. 20 mL of concentrated hydrochloric acid is dissolved in 100 mL of water. Afterwards, pour the reactant into this solution, a considerable amount of powder-like crystal (crude product) is separated out and float on the surface of the liquid. Filtrate the mixture and recrystallize the cake in 40mL of ethanol (Note 2) . 4.0g of colourless acicular crystal (pure product) is obtained. The final yield is 81.4%
1. Ethanol must be added with stirring as quickly as possible. Or the hydroxylamine released will decompose spontaneously.
2. Recrystallizations with ethanol must be carried out on a hot-water bath. Organic solvents like ethanol, aether or something can be ignited easily by flames or sparks.
The order of mixing the reactants requires some further adaption. The decomposition of hydroxylamine must be prevented.
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Procedure
A mixture of 5.0g of diphenylketone, 3.0g of hydroxylamine hydrochloride, 5.0g of sodium hydroxide is placed in a 150mL single-necked flask. Then cover the mixture with ethanol immediately (Note 1) and a few drops of water is added. Heat the flask on a steam bath for 10 minutes. 20 mL of concentrated hydrochloric acid is dissolved in 100 mL of water. Afterwards, pour the reactant into this solution, a considerable amount of powder-like crystal (crude product) is separated out and float on the surface of the liquid. Filtrate the mixture and recrystallize the cake in 40mL of ethanol (Note 2) . 4.0g of colourless acicular crystal (pure product) is obtained. The final yield is 81.4%
Notes
1. Ethanol must be added with stirring as quickly as possible. Or the hydroxylamine released will decompose spontaneously.
2. Recrystallizations with ethanol must be carried out on a hot-water bath. Organic solvents like ethanol, aether or something can be ignited easily by flames or sparks.
Discussion
The order of mixing the reactants requires some further adaption. The decomposition of hydroxylamine must be prevented.
Photographs of the Experimental Operations
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晶体很好看。。。。。
这个物质的用途？？？
这个物质的用途？？？
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额 我一看是肟 还以为是什么糜烂性毒剂呐 把我白激动一场.....
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欢迎！！！ [s:261] 的是现在还没有可以发上去的实验。。。
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做的实验不错……腿好了？我这段时间不去实验室了……有事……你现做啊……
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建议LZ做一下路米诺的。。更震撼一点。。。。。。
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通报一下：昨天我重做了该合成实验，第二步在我的严格监控下终于做出东西来了。由于没有真空泵，过滤花了我一个多小时。
现在那坨湿漉漉的滤饼在干燥器里头，过几天再去重结晶。
现在那坨湿漉漉的滤饼在干燥器里头，过几天再去重结晶。
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生成肟的反应是多种有酮类化合物参与的亲核反应，具有代表性。
从机理上来说，该反应也可以理解为一种 加成—消去 的经典反应。
从机理上来说，该反应也可以理解为一种 加成—消去 的经典反应。
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