lalalympo
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Preperation of isbutyl nitrite
I'm preparing for a synthesis of isobutyl nitrite, I've been gathering information on the chemical and its subcategory; alkyl nitrites.
There are still some things where I'm not sure of regarding the preparation and purification of the product.
First of all is the acid choice, HCl and H2SO4 are commonly used. I happen to have a 1L bottle of technical grade sulfuric acid lying around, but if
there are disadvantages to using sulfuric acid I can order some concentrated hydrochloric acid.
Now in accordance with syntheses I found online, I will cool my acid and nitrite solution in the fridge and keep the reaction vessel in a salt-ice
bath to limit NOx formation.
Onto purification and storage. For the purification I planned on doing a few washes with sodium bicarbonate solution, and dry the washed product with
anhydrous magnesium sulfate to minimize water content. I want to get my product as clean as possible be able to store it, without decomposing, for as
long as possible.
To make the isobutyl nitrate stabler I came across a few methods, namely: Adding glycerin (or glycerol) to reduce water content and absorb
decomposition products, Dissolving the alkyl nitrite in its corresponding alcohol (isobutanol in my case) and adding a drop of concentrated sulfuric
acid to keep the pH on the low side (as suggested by another sciencemadness user). I'm not sure whether the chemicals used in the washing and
stabilization processes affect the isobutyl nitrite.
If anyone has experience on this subject and/or sees flaws, be sure to let me know. All help is appreciated. 
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RobRylan
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What exactly are you going to do with it? Get high?
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Maroboduus
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This from a guy who wants to make thalidomide?
Nobody pestered you by asking, "what are you going to do with it, breed an alternate race to flipper-men?
NOTE: The other recent nitrite thread has advice by Melgar suggesting the use of sodium carbonate to neutralize the residual acids. And also storage
over sodium carbonate for long term stability.
[Edited on 20-1-2017 by Maroboduus]
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RobRylan
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You're right, I retract that comment.
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lalalympo
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Quote: Originally posted by Maroboduus  |
This from a guy who wants to make thalidomide?
Nobody pestered you by asking, "what are you going to do with it, breed an alternate race to flipper-men?
NOTE: The other recent nitrite thread has advice by Melgar suggesting the use of sodium carbonate to neutralize the residual acids. And also storage
over sodium carbonate for long term stability.
[Edited on 20-1-2017 by Maroboduus] |
I hadn't seen that post before, thanks for letting me know.
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thegratefuldead
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This is the other post
http://www.sciencemadness.org/talk/viewthread.php?tid=71858
I would like to know how your stabilization process works!
Id been making Isopropyl, wich is more volatile, washed with Sodium bicarbonate...in this case only the freezer helps..
Now im looking for Butyl, im gonna try the glycerin...
Im using HCL, i have read that H2SO4 works well, but some people recommend HCL instead, i dont know why
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XeonTheMGPony
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HCl is easier to remove from the final product as it is a gas where as sulfuric acid is a viscous oil that likes to stick around!
oldish thread but looking into this stuff for my azide synth for the isopropyle form.
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DrMethyl
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I recommend H2SO4 because you have no risk of breathing HCl if some is left in your final product. But if washing is done properly both are roughly
the same...
By the way using H2SO4 is more exothermic so a better cooling bath is necessairy and slower addition of acid.
Did you plan to test the reaction soon ? Don't forget to post your result, I am very interested. You can also try nitrition of different alcohol and
compare your results : yield and final comparison test of effect. You can try on isopropanol, n-butanol, s-butanol, isobutanol, isopentanol, pentanol,
...
reagrds,
Dr. Methyl
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Praxichys
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Just be careful if you start exploring nitrites of small alcohols. IIRC the dinitrite of ethylene glycol and the trinitrite of glycerol are explosive.
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Amos
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I recommend dissolving the alcohol in a minimal amount of water with good and persistent stirring before the reaction. This (and using a robust excess
of the other reagents) should help to insure that your final product contains as little leftover alcohol as possible.
If your end goal is to inhale it, I wouldn't recommend it. Even just working near it in close proximity has given me a headache, and the inhalation
part just makes that worse.
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