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Author: Subject: Issues with Soxhlet set up
JJay
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[*] posted on 19-1-2018 at 16:15


I think you're making mescaline.



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NEMO-Chemistry
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[*] posted on 19-1-2018 at 21:42


I think your better buying it, cheaper, much quicker. Your way isnt going to work well, i dont think your Mescaline like that though, i think your aiming for black tar crap. But JJay could be right, it could be Mescaline, but me thinks i got him this time! I am 99.9% sure your target with that method is black crap.

Oh and a nice warm house......If your skint how come you can afford a very large amount of ether your going to use?

[Edited on 20-1-2018 by NEMO-Chemistry]
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S.C. Wack
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[*] posted on 20-1-2018 at 09:37


I think he's making people react. If he actually had the nitrostyrene, ether, and LAH, the target is fire.



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[*] posted on 20-1-2018 at 10:25


He's gonna use dry ice and a Graham condenser for ether???
Don't think this poster is exactly lab-savvy.
Don't think he's ever used either ether. (Used ether either, sorry.)

But isn't the point of this modification so you can use less ether to dissolve reactants for the reaction?

If just adding a saturated solution really slowly is all you're after, then break out one of those constant addition funnels.
Those suckers are just worlds apart from regular pressure compensating addition funnels for this kind of thing.




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S.C. Wack
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[*] posted on 20-1-2018 at 11:37


Check the original literature of Ramirez and Burger, and Nystrom and Brown, which is on Rhodium and elsewhere. The pressure equalizing funnel I mentioned earlier is for the side arm which is much like the Soxhlet's.



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[*] posted on 24-1-2018 at 19:15


Ether is nothing to worry about, until you open the bottle
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[*] posted on 26-1-2018 at 15:01


When working with LiAlH4, it is important to be a control freak.

Therein I am not wild about using a Soxhlet in the process. There is the potential for a loss of homeostasis. Since your ether is already refluxing.... How will your LiAlH4, respond to the automatic addition of more reactant? Perhaps, not well.

That being said, I had friends who utilized the Soxhlet/LiAlH4/DiethylEther technique, perhaps 40-50 times, without serious incident. Number 51, was their unlucky number.

A small building disappeared.

It went like this. A Graham condenser cools pretty well, but isn't very good for a reflux like this. Quite possibly, it becomes backed-up with distillate, and it floods.

So, the Soxhlet was outfitted with an Allihin. Which is a decent condenser, but not very good for ether, because it allows too much to escape.

A long uncooled extension tube is affixed to the top of the Allhin, in an attempt to improve ether retention. The tube extends outside, and above roof level. It did not work well enough.

During the hydrolysis stage of the reduction, things got hot, and ether loss reached a critical juncture. There was either no reserve ether, or no way to safely get it into the hot slurry.

Hot ether vapor and hydrogen, vented through the extension tube, fast. Pressure built up. The tube is emitting a loud didgirydoo type sound. This interesting harmonic effect attracts the interest of neighbors, and concerns them enough, that they call the local authorities for reassurance.

My compatriots, courageous young chemists, but no fools.... Exit the building. At just about that time, Public Safety Workers arrive, internal pressure forces the apparatus apart, the building quickly fills with ether vapor and hydrogen gas..... And Kabloouie!

This made the local papers, and arrests were made. Now, the laws were different in those days. And eventually, with the assistance of lots of lawyer money, the fair-haired boys avoided prosecution.

Awful lot of trouble ensued, over a shortage of ether, and lack of an adequate condenser.

If you are gonna run this reaction, either use a high-tech condenser, or have a 24/40 female, welded to the top of your Soxhlet's Allihin. This will allow you to attach an auxillary condensor, and thereby retain yer pretty face.

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[*] posted on 26-1-2018 at 15:11


If you want to get some safer practice in first, distill a gallon of petrol on a camp stove. If you manage that OK then have a go with the synth.
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