Levamisole removal with Hexane Question

[citypress100]

Have read guides online about washing freebase with Hexane and water - most of the information seems to come from the same place.

They say for 1g of freebase use 100ml of Hexane - my question is, do I need 100ml of Hexane for every g of Chang? That seems excessive. Would 100ml of hexane be enough for say 7g?

Any advice would be appreciated.

 

[LucidSDreamr]

Have read guides online about washing freebase with Hexane and water - most of the information seems to come from the same place.

They say for 1g of freebase use 100ml of Hexane - my question is, do I need 100ml of Hexane for every g of Chang? That seems excessive. Would 100ml of hexane be enough for say 7g?

Any advice would be appreciated.

What are the solubility in in mg/mL of levimasole and of cocaine base in hexane?

I feel like they are both going to be too soluble in hexane but I have. I idea you need ti look up those solubilities.

Are you considerinf an acid base liquid liquid extraction with water and hexane ?

 

[LucidSDreamr]

Have read guides online about washing freebase with Hexane and water - most of the information seems to come from the same place.

They say for 1g of freebase use 100ml of Hexane - my question is, do I need 100ml of Hexane for every g of Chang? That seems excessive. Would 100ml of hexane be enough for say 7g?

Any advice would be appreciated.

What are the solubility in in mg/mL of levimasole and of cocaine base in hexane?

I feel like they are both going to be too soluble in hexane but I have. I idea you need ti look up those solubilities.

Are you an acid base liquid liquid extraction with water and hexane ? This might be hard

 

[citypress100]

What are the solubility in in mg/mL of levimasole and of cocaine base in hexane?

I feel like they are both going to be too soluble in hexane but I have. I idea you need ti look up those solubilities.

Are you an acid base liquid liquid extraction with water and hexane ? This might be hard

Yeah this is what I'm trying to find out, but I'm struggling to find the solubility of freebase in hexane anywhere - most posts I've read using this method are using the ratios described in the DEA journal "The Separation of Cocaine and Phenyltetrahydroimidazothiazole Mixtures"

The method is described below (ammended to remove the majority of the irrelevant Ether steps as these were ineffective):

"The cocaine HCl/tetramisole HCl mixture was converted to the base form by dissolving the mixture in boiling water and adding dilute ammonium hydroxide until the solution was basic and precipitation occurred. The mixture was allowed to cool, and the water was removed. The remaining base mixture was allowed to dry overnight.

Ten 50 mg portions were combined with 5 mL of Hexane or Ether in separate 15mL test tubes. All samples were heated at 75'C for approx 5 min. Once the solutions were cooled, 5 mL of water were added to each test tube. The samples were shaken vigorously and centrifuged for 2 min. The solvent layer was removed and washed again with water. The washing process was repeated up to four times."

Hexane boils at 69'C (ether only like 35'c), so I'm assuming the reason for heating the mixture to 75'C is to remove any excess hexane. The mixture was then vigourously shaken in water to "wash it" and repeated multiple times because levamisole is only partially soluble in water, so it takes several efforts to dissolve all of it out of the mixture. I'm assuming that once the cocaine freebase reacts with hexane, it is no longer soluble in water?

So, it seems to be they've used 5ml of Hexane per 50mg of cocaine/levamisole base as a deliberately excessive amount to ensure the freebase fully dissolves. As 5ml:50mg = 100ml:1g, this is what has commonly been discussed as the correct measurements. They also used the same 5mL amount of Ether for the other samples, so the 5mL measurement can't be based on the relative solubities of the substances.

100ml hexane per g of base seems excessive to me, but I'm not basing that on anything factual. If anyone has info on the solubilities of the mixtures involved, I'd be grateful.

I did find this other guide and his suggestions of levels of hexane require seems much more reasonable: https://drugs-forum.com/threads/freebase-cocaine-with-levamisole-removal-steps-pics.352814/

 

[LucidSDreamr]

Yeah this is what I'm trying to find out, but I'm struggling to find the solubility of freebase in hexane anywhere - most posts I've read using this method are using the ratios described in the DEA journal "The Separation of Cocaine and Phenyltetrahydroimidazothiazole Mixtures"

The method is described below (ammended to remove the majority of the irrelevant Ether steps as these were ineffective):

"The cocaine HCl/tetramisole HCl mixture was converted to the base form by dissolving the mixture in boiling water and adding dilute ammonium hydroxide until the solution was basic and precipitation occurred. The mixture was allowed to cool, and the water was removed. The remaining base mixture was allowed to dry overnight.

Ten 50 mg portions were combined with 5 mL of Hexane or Ether in separate 15mL test tubes. All samples were heated at 75'C for approx 5 min. Once the solutions were cooled, 5 mL of water were added to each test tube. The samples were shaken vigorously and centrifuged for 2 min. The solvent layer was removed and washed again with water. The washing process was repeated up to four times."

Hexane boils at 69'C (ether only like 35'c), so I'm assuming the reason for heating the mixture to 75'C is to remove any excess hexane. The mixture was then vigourously shaken in water to "wash it" and repeated multiple times because levamisole is only partially soluble in water, so it takes several efforts to dissolve all of it out of the mixture. I'm assuming that once the cocaine freebase reacts with hexane, it is no longer soluble in water?

So, it seems to be they've used 5ml of Hexane per 50mg of cocaine/levamisole base as a deliberately excessive amount to ensure the freebase fully dissolves. As 5ml:50mg = 100ml:1g, this is what has commonly been discussed as the correct measurements. They also used the same 5mL amount of Ether for the other samples, so the 5mL measurement can't be based on the relative solubities of the substances.

100ml hexane per g of base seems excessive to me, but I'm not basing that on anything factual. If anyone has info on the solubilities of the mixtures involved, I'd be grateful.

I did find this other guide and his suggestions of levels of hexane require seems much more reasonable: https://drugs-forum.com/threads/freebase-cocaine-with-levamisole-removal-steps-pics.352814/

I mean it should work if it’s a published procedure but it’s one of those things you’ll have to actually do using trial and error somewhat until you have fully optimized the procedure for your hands and solvents etc.

Didn’t read the links just what you posted….but what is the mechanism of the separation? Simply solubility in basic solution or ionization of either levamisole or cocaine via protonation (while leaving the other component of neutral charge) and extracting the protonated species out of the mixture in the aqueous phase.

Answering which is these two mechanisms (acid base chemistry or just purely solubility of both basis)….is going to be the information you need in order to guide how you do this.

And you’re best off starting on small test batches first in case something goes wrong

 

[citypress100]

I mean it should work if it’s a published procedure but it’s one of those things you’ll have to actually do using trial and error somewhat until you have fully optimized the procedure for your hands and solvents etc.

Didn’t read the links just what you posted….but what is the mechanism of the separation? Simply solubility in basic solution or ionization of either levamisole or cocaine via protonation (while leaving the other component of neutral charge) and extracting the protonated species out of the mixture in the aqueous phase.

Answering which is these two mechanisms (acid base chemistry or just purely solubility of both basis)….is going to be the information you need in order to guide how you do this.

And you’re best off starting on small test batches first in case something goes wrong

Yeah definitely on board for trial and error, that's half the fun and not expecting perfection on my first attempt, but I'm not understanding the chemistry. With the other washes the chemical processes make sense to me - e.g ethanol and amphetamines - cocaine hcl dissolves in ethanol, whereas amphetamines won't, so that's how they are separated.

Going back to your question about the method - my understanding is the hexane is used to dissolve the cocaine freebase, whilst the levamisole would not dissolve. You then add water, which the levamisole will dissolve in. You then use a centrifuge (or a shit load of hand shaking) as the hexane and water layers are different densities, so you can just extract one layer with a pipette. - you repeat the process because levamisole has low solubility in water, so it takes a few tries to absorb all of it. It would make sense at that point to boil off the Hexane to leave behind just the freebase, with the levamisole washed out.

But I don't understand why you heat the hexane to above it's boiling point right at the start? Even if it dissolves the freebase to start with, surely it doesn't affect the hexane's boiling point?

I asked on another board and someone suggested the test tubes would be bunged to prevent the vapour leaving the tube - perhaps the hexane has to be at a higher tempature to absorb the freebase? I'm not a chemistry expert, but I know temperature can affect solubility levels.

 

[LucidSDreamr]

Yeah definitely on board for trial and error, that's half the fun and not expecting perfection on my first attempt, but I'm not understanding the chemistry. With the other washes the chemical processes make sense to me - e.g ethanol and amphetamines - cocaine hcl dissolves in ethanol, whereas amphetamines won't, so that's how they are separated.

Going back to your question about the method - my understanding is the hexane is used to dissolve the cocaine freebase, whilst the levamisole would not dissolve. You then add water, which the levamisole will dissolve in. You then use a centrifuge (or a shit load of hand shaking) as the hexane and water layers are different densities, so you can just extract one layer with a pipette. - you repeat the process because levamisole has low solubility in water, so it takes a few tries to absorb all of it. It would make sense at that point to boil off the Hexane to leave behind just the freebase, with the levamisole washed out.

But I don't understand why you heat the hexane to above it's boiling point right at the start? Even if it dissolves the freebase to start with, surely it doesn't affect the hexane's boiling point?

I asked on another board and someone suggested the test tubes would be bunged to prevent the vapour leaving the tube - perhaps the hexane has to be at a higher tempature to absorb the freebase? I'm not a chemistry expert, but I know temperature can affect solubility levels.

The heat will just help the coke dissolve…depending how soluble it is you may not need to even heat it though. In fact if cocaine base is very soluble in hexane I would recommend doing everything with very cold solvents so that this will even further discourage the levimisale from dissolving into the hexane and cocaine phase…if it’s the case that levimisale isn’t that soluble in hexane and cocaine is….cooling the hexane is helpful.


If you do end up heating anything be extremely careful not to use an open flame or even sparks around hexane

 

[citypress100]

The heat will just help the coke dissolve…depending how soluble it is you may not need to even heat it though. In fact if cocaine base is very soluble in hexane I would recommend doing everything with very cold solvents so that this will even further discourage the levimisale from dissolving into the hexane and cocaine phase…if it’s the case that levimisale isn’t that soluble in hexane and cocaine is….cooling the hexane is helpful.


If you do end up heating anything be extremely careful not to use an open flame or even sparks around hexane

Thanks for the tip - yeah I can be a little clumsy so hopefully don't blow myself up - I have bought a respirator, safety googles, gloves and my old school lab coat still fits me nicely ha.

Yeah I think you're onto something regaring the solubility, just confused why you heat to over the boiling point of hexane.

Perhaps I'm over-reacting regarding the temperature - like when you boil water, it doesn't all just evaporate immediately as soon as it hits 100'C. So, you keep the test tubes bunged to prevent vapour leak, then the boiling hexane would absorb the freebase more efficiently. Perhaps this is the idea?

Edit: my idea was to buy a water bath so I can control the temperature and also avoid using an open flame.

 

[citypress100]

Fuck, just been on a deep youtube rabbit hole - you do something called reflux using a condenser.

Basically, you heat the hexane, it boils, turns to vapour that rises - the condenser has cold water running through it, so it causes the vapour to cool back to liquid and drip back into the flask.

Learn something new everyday!