Cocaine Loss of product during A/B extraction

[ganandorf]

I recently performed an acid base extraction on 4 grams of coke. After freebasing it with ammonia, the weight was 1.2 grams. Ok, my coke isnt the greatest, but i proceeded. After turning it back into cocaine hcl, the weight aas only 0.6 grams! If anything, the weight should go up because i am adding hcl molecules. Please take a look at what i did and tell me where i went wrong:

When turning the cocaine base into cocaine hcl, i dissolved the 1.2 grams into 18 mL of acetone (the purity of the acetone was 99.5%). In a seperate beaker, i dissolved 0.3 mL of 31.45% pure hydrochloric acid into 0.6 mL of 99.9% pure methanol. While swirling both beakers, i poured the hcl/methanol mix into th
e base/acetone solution. I then let it sit for about 4 hours to allow crystallization. I then uncovered the beaker, scratched the inside of the beaker and stirred a bit to allow more crystallization. At this point, I let it sit for about 4 more hours. When i uncovered the beaker again, there was no more liquid inside. I am guessing that it evaporated.

Note that the ratios i used were 15 mL of acetone per gram of cocaine base and 00.25 mL of hcl acid per 0.5 mL of methanol per gram of cocaine base



Please note that i also performed a standard acetone wash at the very end to get rid of any excess hcl that was on the coke



One second thought, I think I know why this happened and I think it is my fault. The acetone was only 99.5% pure. I used about 50 mL of acetone in the entire process, which means there was about 0.25 mL of water used. This is very bad, considering that cocaine hcl is soluble in about .4 mL of water.

Also, from reading previous threads on acid-base extractions, I should have used a hydrochloric acid that was >= 35% pure. The difference between 35% and 31.45% pure is great when we're talking about a product that is extremely sensitive to water.

But I still ask, are these two reasons the most likely reason why I lost product or was there a mistake in the actual process that I made?

 

[Johnnyfreeman]

The problem im having is that its not crystallizing at all. I added 3g of the product to 30ml of acetone. I then add a hcl:methanol solution to the mix & no reaction took place! I'm really baffled as to what is preventing crystallization. Could any body help at all?

 

[Bambooshoot]

I am sorry I do not have an answer to your question but will give you a heads up that bumping your own threads is not particularly liked here. If you have something to add, edit our post. Bumping your thread will not make people answer any quicker. I thinkyou will get a better response over in ADD now known as Neuroscience and pharmacology discussion. Those guys are awesome. Oh and welcome to Bluelight! ~Bamboo

 

[sekio]

Your cocaine was probably garbage to start with. And it's likely the freebase was not dry... Also, A/B ing small amounts is prone to large (>50 per cent) losses.

If you don't carefully adjust the pH with hydrochloric, you could have also just destroyed the cocaine adding HCl and water and letting it sit.

 

[pbuilder]

How was the high from the .6g's you had left though? Was it actually a whole nother drug like I've heard it is, compared to the cut to fuck stimmy, paranoid shit all over the street?

 

[Johnnyfreeman]

Oh sorry im very new to this! But @sekio i think the stuff was decent. Does it have to be dry? & how would you recommend i add the hcl in order to lower the base more effectively? Do i still use methanol. I need help lol im losing alot of money!

 

[sekio]

"I think the stuff was decent" is not good enough, if you do an A/B and you lose 75% of the mass, you are either spilling it everywhere or your cocaine isn't really cocaine. It needs to be absolutely dry or the water will destroy the ester linkage and inactivate it all.

You probably have to generate gaseous dry HCl if you want to have good recovery (don't do this if you don't know what you're doing, or you will hurt yourself), or add it very very slowly so every drop causes more hydrochloride to flock out and then immediately remove the precipitate and dry it. Again, water plus acid plus cocaine equals no more cocaine. You have to prevent them from "seeing" each other.

 

[Johnnyfreeman]

So on a scale of 1-10 how difficult would this process be?

 

[ganandorf]

"I think the stuff was decent" is not good enough, if you do an A/B and you lose 75% of the mass, you are either spilling it everywhere or your cocaine isn't really cocaine. It needs to be absolutely dry or the water will destroy the ester linkage and inactivate it all.

You probably have to generate gaseous dry HCl if you want to have good recovery (don't do this if you don't know what you're doing, or you will hurt yourself), or add it very very slowly so every drop causes more hydrochloride to flock out and then immediately remove the precipitate and dry it. Again, water plus acid plus cocaine equals no more cocaine. You have to prevent them from "seeing" each other.

Sorry about this very late reply, it's just that no one replied to my thread for so long so I stopped checking up on it.

Anyway, I am trying to understand exactly what you are saying. Please correct me if I am wrong. You are saying that the presence of the water in the hcl (as well as maybe the very slight presence of water in my acetone and methanol) is responsible for destroying some of my coke. Thus in order to prevent a loss of coke due to water, I cannot let the coke and water "see" eachother, i.e. I cannot allow them to react. In order to do this, as soon I add a drop of hcl, I must remove whatever precipitates and allow it to dry. While it's drying, I add another drop of hcl and remove the precipitate and continue in such fashion until further drops of hcl no longer produce a reaction. Once the further addition of hcl into the cocaine base/acetone solution no longer produces anymore crystals, then everything I put aside is my total yield.

Is this correct?


EDIT: I just realized that cocaine hcl is soluble in methanol. Is the presence of methanol a problem? Surely this must be resulting in some loss of yield....according to a source I just read, the two solvents, let's call them A and B, that I use to convert the cocaine base to cocaine hcl must fulfill these requirements:

1) Cocaine base must be soluble in solvent A
2) solvent B must be miscible with hydrochloric acid
3) Cocaine hcl must be insoluble in a mix of solvent A and solvent B.

If this is true, then I am pretty sure that while acetone is a decent choice for solvent A, methanol is a poor choice for solvent B. Do you have any suggestions what I can replace the methanol with?

 

[tricomb]

The reason I prefer anhydrous acetone washes over A/B extractions especially with cocaine, (not that I use this drug anymore, lost interest a long time ago) is:

A) you're cocaine is likely garbage as global cocaine purity levels are in the shitter.

B) you don't lose as much product, assuming there IS desired product amongst that white, cocaine-like powder that is more likely to be baking soda + levamisole + prilocaine/procaine/benzocaine/other non-cocaine numbing agents.

If you were trying to freebase like, a kilo, I can understand going the extra mile with an A/B extract but for personal use, acetone (anhydrous) works better.

 

[sekio]

Cocaine plus acid or base plus any alcohol, or water = destroyed cocaine through hydrolysis/transesterification. Heat makes this reaction go faster. Methanol, ethanol, water are all bad solvents for this reason.

Ideally you need to suspend the cocaine base in a nonpolar solvent that is only minimally miscible with water (ether) and add dry hydrogen chloride as a gas or solution, not aqueous hydrochloric acid. Generating and handling gaseous hydrogen chloride is an excellent way to get yourself killed if you don't have the requisite fume extractors...

Acetone plus HCl will result in water being formed because acetone undergoes an acid-catalysed aldol condensation so it's not a really good solvent for an A/B.

The other way around this is adding the acid, SLOWLY, dropwise, to your cocaine base in solution, not the other way around, and watching the pH carefully....

 

[tricomb]

isn't refined petroleum (another extremely explosive and volatile collection of liquid energy in the form of hydrocarbons, distilled and homogenized with octane boosters like benzene etc) a commonly used non-polar agent for cocaine purity testing? Or rather just at the coca plantations processing facilities..., I don't remember right now but the only people I knew who dealt in only the best, highest quality cocaine mention using gasoline prior to making freebase and/or adulterating HCl 50/50 for resale.

 

[sekio]

Gasoline is used at the coca plantations to produce crude cocaine base, because it's a cheap and readily availiable nonpolar solvent. Getting gasoline in the jungle is easy, getting VM&P naptha or diethyl ether is much harder.

It's not something people should hold as a mark of quality.

 

[ganandorf]

Cocaine plus acid or base plus any alcohol, or water = destroyed cocaine through hydrolysis/transesterification. Heat makes this reaction go faster. Methanol, ethanol, water are all bad solvents for this reason.

Ideally you need to suspend the cocaine base in a nonpolar solvent that is only minimally miscible with water (ether) and add dry hydrogen chloride as a gas or solution, not aqueous hydrochloric acid. Generating and handling gaseous hydrogen chloride is an excellent way to get yourself killed if you don't have the requisite fume extractors...

Acetone plus HCl will result in water being formed because acetone undergoes an acid-catalysed aldol condensation so it's not a really good solvent for an A/B.

The other way around this is adding the acid, SLOWLY, dropwise, to your cocaine base in solution, not the other way around, and watching the pH carefully....

I can't work with ether or dry hydrogen chloride gas. Too dangerous for an amateur like me. I will have to work with a concentrated aqueous hcl solution. I have a couple questions if you could please answer them...

Would using toluene as my nonpolar solvent work? Cocaine base is freely soluble in it, and it is only very slightly miscible with water. Plus cocaine hcl is obviously not soluble in it. Also, what is the function of the polar solvent that I mix with the hcl acid? Why can't I just add my concentrated hcl acid (my bottle says 36-38 % ) dropwise into the base/toluene solution until cocaine hcl stops precipitating?


EDIT: Would adding hcl acid by itself not work because it's not very miscible with the toluene?

 

[sekio]

The problem you will run into is that because cocaine HCl is so soluble in water, when you add ~37% HCl, that forms an aqueous phase that all your cocaine hydrochloride goes into, and it's also where any remaining acid will prefer to reside. Really you have to try to remove all the water from this to ensure you get the best yields.

Also, what is the function of the polar solvent that I mix with the hcl acid? Why can't I just add my concentrated hcl acid (my bottle says 36-38 % ) dropwise into the base/toluene solution until cocaine hcl stops precipitating?

You don't need another polar solvent. In fact it is detrimental... That's exactly what you should do. Use vigorous mixing when you add HCl. But you'll probably have to measure the pH of the water frequently so it doesn't get too acidic rather than watching for a precip. Don't be suprised if you don't see very much of a precipitate, or it redissolves. After the water solution is very slightly acidic, remove the water phase & any precipitate from the toluene and then evaporate it gently.

 

[ganandorf]

The problem you will run into is that because cocaine HCl is so soluble in water, when you add ~37% HCl, that forms an aqueous phase that all your cocaine hydrochloride goes into, and it's also where any remaining acid will prefer to reside. Really you have to try to remove all the water from this to ensure you get the best yields.



You don't need another polar solvent. In fact it is detrimental... That's exactly what you should do. Use vigorous mixing when you add HCl. But you'll probably have to measure the pH of the water frequently so it doesn't get too acidic rather than watching for a precip. Don't be suprised if you don't see very much of a precipitate, or it redissolves. After the water solution is very slightly acidic, remove the water phase & any precipitate from the toluene and then evaporate it gently.

Damn, the more I learn about this specific reaction, the more I hate water...

I called my chemical supply company today and they said they won't be able to get me toluene or hexanes (the C of A says it is a mix of 5 isomers, and it seems like this is also a suitable nonpolar solvent to use), so I am going to go ahead and salt the base I currently have (2.75 g) using the method I originally posted. The only difference will be that the acetone and methanol are both ACS grade this time, and the hcl acid is 36-38 %. I will also evaporate the mother liquor after precipitation is done (if I do indeed get something precipitating) to see if I get anything left over.

I will attempt to crystallize the cocaine base out of just toluene (the hexanes mix) and hcl acid in a few weeks once I get the required chemicals.

A quick couple questions:

1) When I use the acetone/hcl/methanol method, should I remove any precipitate as soon as I see it and dry it off? Or leave it in there and as soon as the pH of the water hits about 6 - 6.5 should I remove what I currently have, and then evaporate the mother liquor without making it more acidic?

2) I understand that when I do use the toluene, I will add concentrated hcl by itself. But how come when I am using acetone to dissolve the base, I have to mix the methanol with the hcl? Does it have something to do with acetone being polar and as an exception, dissolves the cocaine base?

 

[sekio]

I would not use any method that had methanol/acetone in it (except as a wash). Cocaine HCl is soluble in methanol, so is the base to an extent. Not only that but methanol will react with cocaine in the presence of acid (destroying it), as well as acetone reacting with itself in the presence of acid to form aldol condensation products and more water. It's a non starter.

Erowid has an Ask Erowid page on the topic, they say dissolve cocaine in your light naptha or ether and add HCl in isopropyl alcohol. VM&P naptha is a suitable substitute if you can get it. Also, Bestine (heptane) from art supply houses, used as a paintbrush cleaner.

The way I would do this is, figure out how much HCl you're going to need to add, add that much aqueous HCl to some isopropanol, and dry the resulting wet solution as best as you can with oven baked magnesium sulfate (Epsom salts), to basically make a solution of dry HCl in 99% isopropanol. Then add that dropwise to your cocaine in naptha (dried the same way), and just collect the precipitate as it falls out. I don't think cocaine HCl is soluble in small amounts of isopropanol plus large amounts of hexane/naptha.

Don't use toluene if you can help it, the shit takes forever to evaporate. Really, if you're going to do this, take the time to do it right rather than half assing it.

If your chemical supplier won't sell you hexane or toluene, you must not look very legit either...

 

[Jktm]

Couldn't they just gas it with HCl after they have the base sitting in their solvent at the end of it all?

 

[sekio]

I can't work with ether or dry hydrogen chloride gas. Too dangerous for an amateur like me.

It's kind of advisable... if you don't have a good gas generator setup, a fume hood, and scrubbers... you can seriously harm yourself.

 

[ganandorf]

I would not use any method that had methanol/acetone in it (except as a wash). Cocaine HCl is soluble in methanol, so is the base to an extent. Not only that but methanol will react with cocaine in the presence of acid (destroying it), as well as acetone reacting with itself in the presence of acid to form aldol condensation products and more water. It's a non starter.

Erowid has an Ask Erowid page on the topic, they say dissolve cocaine in your light naptha or ether and add HCl in isopropyl alcohol. VM&P naptha is a suitable substitute if you can get it. Also, Bestine (heptane) from art supply houses, used as a paintbrush cleaner.

The way I would do this is, figure out how much HCl you're going to need to add, add that much aqueous HCl to some isopropanol, and dry the resulting wet solution as best as you can with oven baked magnesium sulfate (Epsom salts), to basically make a solution of dry HCl in 99% isopropanol. Then add that dropwise to your cocaine in naptha (dried the same way), and just collect the precipitate as it falls out. I don't think cocaine HCl is soluble in small amounts of isopropanol plus large amounts of hexane/naptha.

Don't use toluene if you can help it, the shit takes forever to evaporate. Really, if you're going to do this, take the time to do it right rather than half assing it.

If your chemical supplier won't sell you hexane or toluene, you must not look very legit either...

Lol, I meant to write that they won't be able to get me the toluene and hexanes until a few weeks from now.

I like the above method that you posted. I won't have to worry about the magnesium sulfate reacting with the HCL acid, right?

And can you please explain to me how I can figure out what amount of HCL should be added to what amount of ispropyl per gram of cocaine base? I think it has something to do with the molar mass of each substance?

I shall be picking up the VM&P Naptha today or tomorrow and conducting this experiment on Sunday. I will keep everyone updated as to how this experiment goes.