Cocaine A simple method from a paper to separate cocaine and levamisole/tetramisole

[creamynebula]

I just read a paper (The Separation of Cocaine and Phenyltetrahydroimidazothiazole Mixtures, Microgram Journal, Volume 10, Number 2) that showed working methods to separate cocaine HCl from tetramisole/levamisole HCl, two of the methods described are liquid-liquid extractions and thus can be performed by anyone!

Materials:
Water (distilled if possible)
Ammonium Hydroxide solution (paper doesnt say, probably 28% then) (only for method 1)
Paper Filter
Hexane
Heating plate with temperature control
Beakers
Round-bottom glass
Separation Funnel
Cocaine+tetramisole/levamisole

The one that yielded best results:

Convert material to base form by in a beaker dissolving the mixture in boiling water and adding dilute ammonium hydroxide until the solution is basic and precipitation occurs.
Allow the mixture to cool, then remove the water (pour in another beaker through a filter to hold the mixture).
Allow the remaining base mixture to dry overnight. In a round bottom glass combine the mixture with hexane (5mL hexane for each 50mg of material)
Heat at 75ºC for approximately 5 min.
Once the solution cools, add 5mL water for each 50mg of material.Shake vigorously for as long as you have the patience to, in the paper they shaked a bit and then used a centrifuge for 2min.
Remove the solvent layer and wash again with water, repeat the washing process up to four times, more washes will yield purer product.
After you have made the amount of washes you decided to, evaporate the solvent to dryness.
On the procedure descvribed in the paper, in the 85:15 and 70:30 mixtures, tetramisole was COMPLETELY removed (confirmed through FTIR and GC/FID analysis) from the hexane after washing with water five times due do its preferential solubility in water. In the 50:50 mixture cocaine 99+% was obtained.
They tried the same procedure with ether instead of hexane too but it was unsuccessful.

Table with the exact results for this method

# Washes / % cocaine base achieved
(85:15) (70:30) (50:50)

1 94.4 84.3 77.0
2 97.9 93.5 88.2
3 99.2 97.3 95.8
4 99.7 99.1 98.5
5 100.0 100.0 99.4

So generally 2-3 washes at the last step is good enough I think, your cocaine probably wont have more than 5-15% levamisole/tetramisole at start, but rather other cuts, so you may want to do a acetone wash before this procedure to remove those.

 

[creamynebula]

The other one:

Materials:
Water
Chloroform
Round-bottom glass
Heating plate
Cocaine + leva/tetra

Dissolve each 50mg of cocaine/tetramisole mixture in 1mL water in a round-bottom glass [again since unlike in the paper your mixture is likely not only cocaine+tetramisole, if some material does not dissolve in the water remove it through filtration], add 5mL of chloroform for each 50mg of material and shake vigorously for a while. Separate the two layers with a funnel, evaporate the chloroform layer. The resulting solid will be your cocaine, but this method although will produce very pure product will also lose a lot of cocaine, since cocaine is very soluble in water. You can then keep extracting cocaine from the water with chloroform if you wish, you are going to use a lot of chloroform though.
The purity of cocaine isolated from this extraction was >= 90% on average, between all three HCl mixtures.

Table with exact results

% Cocaine HCl achieved
(85:15) (70:30) (50:50)

98.4 95.3 89.3

 

[creamynebula]

In either procedure since in your case your mixture is likely not only cocaine+levamisole like in the paper, if at the very first step when you add water something doesnt dissolve, filtrate this solution to remove this non-water soluble cut.

 

[creamynebula]

Here the better method written in a simpler manner for beginners:

1. Mix 1g cocaine and 20mL water, filtrate insoluble purities. Now heat it till below boiling point, stop heating and proceed immediately.
2. Add amonium hidroxide until precipitation occurs, stop adding when a next drop is not forming more. The precipitate formed is cocaine+levamisole freebase.
3. Allow it to cool, throw water away recovering the solid. If it was cut with ephedrine you just got rid of it with that water. Let solid dry overnight.
4. Mix the solid with 100mL hexane, heat at 75ºC or so for 5min. Let it cool and move to a (separatory) funnel.
5. Add 100mL water, shake vigorously to mix, then stop and let it rest so it separates in 2 layers again. Discard water layer in the bottom
6. Repeat 5. one to three times to improve purity
7. Evaporate hexane, result is cocaine freebase with no levamisole.

To snort here are instructions on how to turn your cocaine base back into cocaine hcl: https://www.erowid.org/ask/ask.php?ID=3151

 

[sekio]

unfortunately you need a source of anhydrous (dry) gas HCl to make HCl in isopropanol as erowid suggests... which makes the operation of salting it out again kind of dangerous.

It probably is best if you add a step where you dry the hexanes with anhydrous magnesium sulphate or w/e, too. Just to minimize water contamination.

 

[fakoni]

Could u plz explain why anhydrous hcl gas?
If.anhyd hcl gas then there is no need for ethanol/methanol at all,right?
Just gas the diethylether until no more flakes are forming?
THX

 

[Fractality]

Could one substitute heptane for the hexane? Aside from tetra/levamisole and ephedrine, what other adulterants are removed with this process?

 

[Fractality]

It probably is best if you add a step where you dry the hexanes with anhydrous magnesium sulphate or w/e, too. Just to minimize water contamination.

Is 95% anhydrous hexane good enough?

 

[Fractality]

Can someone critique the following technique to turn the base back into HCL?

Add distilled water to the base (as little as possible i.e., a few ml). Take a few ml of muriatic/hydrochloric and put in a separate flask. Add a few drops of water to the acid. Now take the acid and add it dropwise into the flask with the base in it. You should notice the base start to disappear. Keep doing this into the base disappears into the solution. Filter this solution and then evaporate it on a pyrex dish (sped up with fan or heat lamp).

 

[Jekyl Anhydride]

From what I remember, the use of water causes a decent portion of the cocaine to convert to benzoylecgonine through hydrolysis.

 

[Fractality]

What if the end result salt form actually has a greater yield than the original base (implying the addition of the HCL molecular weight)? Wouldn't that mean most of the coke is not lost?

 

[Jekyl Anhydride]

A greater yield possibly (Molecular Weight 303 base vs 339 for the HCl), but an increased amount of coke would equate to alchemy. The HCl would be around 0.89 to the base's 1.0

Cocaine readily decomposes to BZE even at neutral pH, and more rapidly in strong base and strong acid, as is typical of most organic esters.Cocaine is unstable in blood and in solution, and is quickly hydrolyzed to benzoylecgonine (BZE) and ecgonine methyl ester (EME), and then finally to ecgonine.

https://www.sciencedirect.com/topics/medicine-and-dentistry/benzoylecgonine

 

[Fractality]

A significant amount of cocaine must remain in water because if you consume it after dissolving it in water, it produces effects. So if the water and acid solution is evaporated within several hours, perhaps enough cocaine remains in the solution to be salted out? This resonates with what I've heard and read elsewhere; that cocaine slowly decomposes in water.