thors.lab
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Synthesizing Nitrobenzene [Video]
Hi,
I've made a new video on the synthesis of nitrobenzene. As always, please check my signature for the link to the video.
Please let me know of any improvements I could have made to the procedure, video editing, narrating, and safety.
If anybody has any idea why the yield was relatively low (64%) please share.
I plan to make phenylhydroxylamine next, then p-aminophenol, then acetaminophen. However, this will have to wait as I've moved and didn't bring my lab
equipment yet.
If you have suggestions for other videos, let me know!
Thanks,
Thor
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Ynzept
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T. Davis: "The nitration of m-dinitrobenzen is too expensive of acid and heat for practical application, and the yields are poor. Toluene and
chlorobenzene are nitrated more easily and more economically, [...]. "
So you could try chlorinating your benzene first or nitrate toluene, then oxidize by means of chromic acid in sulphuric acid solution.
Hope this helps
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Herr Haber
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I'm still waiting for someone to synthesize acetaminophen from willow bark or crude oil 
Absolutely pointless of course but nowadays people snort cinnamon as a challenge...
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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thors.lab
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Quote: Originally posted by Herr Haber  | I'm still waiting for someone to synthesize acetaminophen from willow bark or crude oil
Absolutely pointless of course but nowadays people snort cinnamon as a challenge... |
I have most of it planned out besides the last step — i can’t figure out how to get my hands on acetic anhydride for p-aminophenol ->
acetaminophen
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Cactuar
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Instead of doing 2 water washes I would do one with saturated NaHCO3 and one with brine. This would minimize the amount of product dissolved in the
aqueous phase and reduce the amount of drying agent needed. I would also dry the product before distillation. And looking at the product at 4:27 it
looks like the MgSO4 is moving like a sludge at the bottom of the flask, this tells me it's not really dry. It should be like a hard cake with small
amounts powdered MgSO4 swirling around freely and refusing to "aggregate" with the others.
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thors.lab
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| Quote: Originally posted by Cactuar | | Instead of doing 2 water washes I would do one with saturated NaHCO3 and one with brine. This would minimize the amount of product dissolved in the
aqueous phase and reduce the amount of drying agent needed. I would also dry the product before distillation. And looking at the product at 4:27 it
looks like the MgSO4 is moving like a sludge at the bottom of the flask, this tells me it's not really dry. It should be like a hard cake with small
amounts powdered MgSO4 swirling around freely and refusing to "aggregate" with the others. |
These are great suggestions! Thank you!
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DavidJR
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You used rather a lot of magnesium sulphate, which probably contributed to the yield. I'd use a smaller amount and add more if needed until the
supernatant becomes clear.
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monolithic
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Nice job. I really enjoy the cost analysis at the end of your videos.
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icelake
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| Quote: Originally posted by thors.lab | | I have most of it planned out besides the last step — i can’t figure out how to get my hands on acetic anhydride for p-aminophenol ->
acetaminophen |
Can you try this method?
https://archive.org/download/ChemPlayer/Acetic%20anhydride%2...
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thors.lab
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| Quote: Originally posted by DavidJR | | You used rather a lot of magnesium sulphate, which probably contributed to the yield. I'd use a smaller amount and add more if needed until the
supernatant becomes clear. |
I tried to go little by little, I suppose I had a lot of water left because of the mistake during distillation. :/
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