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Author: Subject: New Video-Synthesis of Nitrophenol
Bmoore55
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[*] posted on 9-4-2022 at 10:15
New Video-Synthesis of Nitrophenol


I am doing my best to stick to what I said I would do. Here is video on the synthesis of Nitrophenol using Nitric Acid and Phenol followed by analysis with NMR and FT-IR. Hope you all enjoy!

https://youtu.be/viLwdmQi9dQ
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Texium
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[*] posted on 9-4-2022 at 18:33


Excellent video! Cool to see a benchtop NMR in action. A couple minor critiques:

-I highly recommend you get a bump bulb for your rotovap. It'll save you a lot of pain by making it easier to recover product and keeping you from having to take apart and clean the whole system whenever it bumps.

-There's two good ways you could get rid of excess water from your product. The cheap way would be to leave it on the filter for a longer period of time and then put it in a flask under high vacuum for an hour or two. Since you have a rotovap, you could also dissolve it all in an organic solvent, dry it over magnesium sulfate, then filter and evaporate it again to get dry crystals.

-You used SO much deuterated chloroform when you made your sample! :o

Those spectra look really great though! I'm pleasantly surprised that it's so easy to get pure o-nitrophenol. I don't think I ever watched ChemPlayer's version, so I wasn't aware that the steam distillation was that selective. I would have also expected more over-nitration to occur, even at the lower temperature. It would be really cool to see an attempted extraction of that tar, since 60+% of the material is probably in there and it probably contains a considerable amount of p-nitrophenol.




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Bmoore55
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[*] posted on 9-4-2022 at 19:09


Hey Texium! Thanks for the input!

I do have a bump flask for the rotovap, I was just a little too excited about finally getting to use it in a video that I kinda got ahead of myself. Having to clean the rotovap was the punishment for my eagerness.

As for the water I did not realize this until after the fact, but the desiccant was spent in my desiccator. I wasted a bunch of time thinking I was making the sample dry when I was really just keeping it wet. Also, you are 100% correct I way overdid the deuterated solvent. I guess I got a little carried away and let this new lab and all this other stuff go to my head haha.

I highly recommend the Chemplayer video, it is a great walk through of this synth.

https://www.bitchute.com/video/bRTGX7mzxrKs/

Thanks again and hopefully I can have some more stuff coming soon.
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Texium
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Herr Haber
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[*] posted on 10-4-2022 at 06:38


Excellent video !
When I wasnt just smiling I was eyes and ears wide open learning.

"Oops" beaker.
Ah, so they have a name :)
"Not to brag"
I kinda knew what you were going to say next but as a hobby chemist I dont need nor have ever considered using a rotovap so I never thought of using one for fractional distillation by changing pressure and not temperature. Your explanations were very interesting.

Your preparations and explanations around the NMR were exactly the kind of content I was hoping for after reading your post some weeks ago.
I didnt understand everything but that's exactly the reason why I am interested in the first place: I know I dont know much !
For me, again as a hobby chemist with no degree in chemistry sample preparation doesnt go a lot beyond weighting, putting in solution or grinding in the ball mill / mortar etc.

Thank you very much, I enjoyed every minute of the video and I'm convinced the next ones will be equally interesting !




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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crow6283
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[*] posted on 10-4-2022 at 07:06


Cool dude! I like your videos keep up the good work.

If you are open to suggestions for content… I really like the format that chemplayer uses sometimes, that is to say … picking a substrate and a target product and trying different methods to get there. Of course they flew a little too close the sun it seems but I think for the hobby chemist (organic) this is the most interesting and useful type of content. Probably not so if you have hopes of making money of your channel.
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[*] posted on 10-4-2022 at 10:46


Bmoore55 very well done!
I fought the steam distillation of orto isomer too. I used my condenser with the widest inner tube diameter I had at hand. I rather did not use the vacuum take off adapter at all due to its narrow tube.
Separation of the para isomer from the remainder in distillation flask was quite tricky. I succeeded with repeatedly partially dissolving the tar in warm 1 % HCl and cooling the solution down. It had to be repeated a lot of times and always only part of the product dissolved and crystallized. Reusing the mother liquor as the solubility is approximately the same as the amount of product crystallized out. Because of reusing mother liquor the later portions were more and more discolored. Crystals usually formed only when cooling down from approx 40 C to 10 C - when cooling down too hot and too concentrated solution there were no crystals but the product just oiled out. Finally crystallizing from 0,5% Na2S2O5 helped to obtain colorless para nitrophenol.
https://www.sciencemadness.org/whisper/viewthread.php?tid=15...




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Bmoore55
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[*] posted on 11-4-2022 at 07:47


Quote: Originally posted by crow6283  
Cool dude! I like your videos keep up the good work.

If you are open to suggestions for content… I really like the format that chemplayer uses sometimes, that is to say … picking a substrate and a target product and trying different methods to get there. Of course they flew a little too close the sun it seems but I think for the hobby chemist (organic) this is the most interesting and useful type of content. Probably not so if you have hopes of making money of your channel.


I am planning on doing just this very thing. I have always felt like there are a lot of experiments which have been attempted in the amateur community and they just did not have the analytical tools to figure out exactly what their reaction did.
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crow6283
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[*] posted on 11-4-2022 at 09:24


Yes that’s absolutely true. I’m glad you have an FT-IR , I mean NMR is great but pretty much out of the reach of an amateur. IR on the other hand… well they’re out there. I myself recently found one… not that I have libraries for it or the slightest clue how to use it.
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