Amphetamine purification by acid-base extraction

ACAB

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Finally something done right :D
 

BakingBread

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what if the product is cut with caffeine?
Would this extract along with the amphetamine, as caffeine sulfate/phosphate?
If so, how much of this would come over? the whole lot?
Thanks!
 

ACAB

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If the amphetamine sulfate is stretched with caffeine and you perform an A/B extraction, due to the solubility of caffeine in water, after adding NaOH and forming a second layer of freebase, most of the caffeine would separate from the amphetamine and remain in the aqueous layer.
 

Beeber

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Can I switch from sulfates and phosphates to hydrochloride? What should I do?
 

UWe9o12jkied91d

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Easy, follow above procedure and replace the acid in the end.Amph. HCl is hygroscopic and will spoil fast, not something you do, unless you wanna smoke it on the spot.
 

Beeber

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Can I do this? Can you explain to me?

1. You must obtain 1 mol of amphetamine-free base (1) by adding amphetamine salts to a 20% NaOH aqueous solution to pH 12, mixing for 15 min and extracting. Amphetamine-free base by DCM or gasoline ether 3 x 75 ml.

2.HCL gas bubbles
 

G.Patton

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Hello. Yes, you have to barbotate HCl gas through amph free base solution
 

Charlie3

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For Point 6. Combine the extracts. Does it mean to combine both the top and bottom layers again? Im confused sorry for the newbie question
 

G.Patton

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It is sort of extraction. All petroleum ether extracts are combined together after 3x extractions.
 

Charlie3

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After ive added petroleum ether 3x times. This is what ive got. So from here, going into step 7, i add mgSO4 into it, seal it and place it in the freezer?
 

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G.Patton

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Have you separated layers after ether addition?
 

Charlie3

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Not yet, right now theres 2 layers that i can see. The petroleum ether is on top. So now i have to remove the petroleum ether first at the top?
 

Charlie3

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Okay got it. Read on it now.
 

JuanoImano4378

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@G.Patton I added amph to water with a 1:1 ratio as your guidelines here and my top layer is transparent. Does transparency indicate purity or less pure?

Also I touched the solutions out of curiosity and noticed that my bottom layer has an oily texture whereas the top layer dries upon contact like alcohol. I used Petroleum Ether to separate the layers but I’m a little bit confused because of the texture.
 

G.Patton

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Hello, amph sulphate is dissolved completely in water. I don't know what did you get as top layer, it isn't amphetamine. Petroleum ether isn't soluble in water and won't extract amphetamine salt. You have to separate this admixture oil and get amph free base with NaOH aq solution addition. Then, you can extract the base by Petroleum ether. Hope you'll understand me well.
 
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JuanoImano4378

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I proceeded to follow the rest of the step as outlined and I managed to get purified amph salt back. It's probably because I put a small amount of amph salt to test out this extraction procedure. I do have one question for the last step though, as I add H2SO4 the amph salt started to crystallize, I tested a small sample by adding more sulphuric acid than supposed to just to see what would happen. The crystals disappeared and it turned into a red-colored solution.

if I don't add enough H2SO4, then some crystals won't crystallize whereas if I add too much, it disappears and becomes red. So question is, how do I know how much H2SO4 to add for maximum yield?
 

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G.Patton

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Hi. Use pH indicator paper. If you don't know about it, look around Lab FAQ section.
 

UWe9o12jkied91d

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If only there was a standardized measurement of acid conc. in solution that you could test for instantly and easily, damn, what a shame, someone should invent this.
 
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