xylene in acid-base extraction of amphetamine

mithyl2

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can xylene be used in place of petroleum ether when doing an acid-base extraction of amphetamine?
 

blacky2340

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Most likely, but it can only be evaporated
 

blacky2340

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As in talking with DMT extraction experience. Both are non-polar solvents. But xylene does leave a bit of residue and has to be evaporated, while petroleum ether lets you freeze the crystals out, also xylene has a smell. I think for your purpose you should try another solvent. Most paint thinners are actually made from petroleum ether, just google the ingredients of each.
 

Osmosis Vanderwaal

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Yeah I'd shy away from xylene and use naptha Did you know that xylene is dimethyl benzene? It is and those methyls aren't hard to knock off and then you have radical methyl ions floating around which could do unexpected things, like the alkylate amphetamine, but probably not on the nitrogen, probably on the phenyl or the alpha or beta 2- methyl-amphetamine anyone? 3-methyl? Paramethyl?
 

mithyl2

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the problem is that ether isn't available where i am and is of course highly volatile. i couldn't really see much of an alternative either. but i do have naptha. i'll try naptha and see how it goes.

i actually tried doing a micro scale acid-base extraction with xylene but i couldn't get the amphetamine to precipitate at the end.
 

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You can try xylene but I'm not sure that it will works. Know for sure about diethyl ether, dioxane, DCM.
 
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mithyl2

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i'll be taking Frit Buchner's advice and trying out naptha in place of diethyl ether.

in the absence of sulfuric acid, when it comes time at the last step to precipitate the amphetamine, is phosphoric acid ok to use? or is hydrochloric better? or something else?

(i'll be using amphetamine that was precipitated during synthesis using phosphoric acid, if that's relevant.)
 

G.Patton

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Naptha is okay, almost the same as PE. Yes phosphoric acid is okay. Hydrochloric acid is not okay =) Read my topic about Amphetamine salts.
 

mithyl2

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what would you recommend i do to get pure naptha? is there a specific petroleum product/cas number i should be looking for?
 

G.Patton

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I don't know what solvents are available in your location. Naphtha is naphtha. Just search it. All of them are okay. The lighter fraction, the easier to evaporate it after.
 

mithyl2

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i'm in uk. i assumed there would be some impurities in store bought lighter fluid for exmample, and perhaps would need a fractional distillation.

for some reason naptha is a bit elusive over here, so wondered if maybe something more readily available such as a type of white spirit (e.g. stoddard solvent, cas no: 8052-41-3) would be suitable instead?
 

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Yes, you can try this one.
 

Osmosis Vanderwaal

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Even with the naptha you'll want to make get it cold to precipitate
And obviously if it has any water in it, it won't precipitate ( so you have to gas it instead of hydrochloric acid) or you can evaporate the naptha. I am not 100% positive of all of this related to amphetamine. I have never seen amphetamine in my life. This is all true related to meth. I suppose you'll be trying to precipitate the sulfate🤔
 

mithyl2

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do you mean gassed with hcl gas?
 

Osmosis Vanderwaal

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I did, but like I said, amphetamine automatically turns to methamphetamine in my head because there is no amphetamine here. The sulfate is the Lewis acid you want not the hydrochloride
 

mithyl2

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i'll be using phosphoric acid to precipitate for the time being as sulfuric is hard to get here.

could you elaborate on what you meant when you addressed a lewis acid as being what i want instead of hydrochloride? i had a quick look on a search engine but couldn't get much more than it forming a lewis adduct. (still very much a noob in chemistry).
 

Osmosis Vanderwaal

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Rather than try to explain it, I'll represent it visually.
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C86p9BPZkI
 

mithyl2

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thank you.

i'm clearer on what a lewis acid/base is, but in the context of precipitating the amphetamine at the end of the acid-base extraction, which acid would it be best to use in place of hydrochloric?

sorry if i'm missing something.
 

Osmosis Vanderwaal

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I guess you are missing prior art, or prior work or...industry standards. Your not missing it. But you think you are. 9/10, people do something a certain way for a reason. Often it's knowledge or experience. Not always but often. There's a reason why amphetamine is made a sulphate. I don't know what it is, but there was a thread aboutv6 weeks ago where someone was asking why amphetamine is most often a sulphate. It could be several acid salts, at least, but sulphate is the goto for a reason I either didn't lookat or forgot
 
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