Can cocaine even more purified by re oxidation ?

[DanTheMan]

Hi,

currently i'm struggling with finding a decent source. Even after
1.Aceton Wash
2.Ethanol Recrystallisation (i speed up the filtration with vaccum could that be a problem?)
3.Convert to Base
4. Hexan L-L Wash
5. Convert to HCL Again
6. Second Ethanol wash
I end up with at least 4 very different looking crystalls.... Color Tests still give unclear reaktion due presence of many diffrent indegrients. Even Water washes won't help.
So i've read a lot about the topic and came to the questions what would happen if i treat the HCL like leaves in production?

I mean
1. Dissolving in alkine soulution to get base
2. Add benzen or kerosen
3. remove water and add sulfiric acid + sodium carbonate
-> i get the paste
4. Add paste to sulfuric acid and water
5. add potassium permanganate (i hope to break down everything beside cocaine)
6. Form to base again via ammonia hxdroxid
->base
base to hcl should be clear.


Would that work ? Has anyone ever tried it?

 

[Osmosis Vanderwaal]

This is all far too convoluted. It's way over the top. I'm pretty confident that you have no idea what you are doing. That is based solely on your choice of verbiage and what information you didn't include. I'm a pretty decent crystsallographer, let's see the crystals. Are you using a multi solvent recrystallization? I can give you a scheme that will actually leave practically no trace of adulterant, but it won't use kerosene or benzene. It definitely won use sodium sulfate that you are making for an unknown reason . Are you checking your ph as you do all this sciencing? Cocaine is a sensitive molecule and there's 100% chance you are breaking it

 

[Osmosis Vanderwaal]

Post your reagent color test results.

 

[DanTheMan]

Okay, i'm unsure about the Ehrlich reagent. It is not supposed to become green... The other give mixed signals.

 

[DanTheMan]

These and some more are all cleanings teks you can find on the internet. But you right i've no idea what happen on molecular level. I'm not a chemist. But i realy like learing alll these things and get rewarded with good blow. Actually i spend more money on eqipment and chemicals than i want to admit. I've read so many sience articeles and patent that i came to the conclusion that this would be possible. The way i descriped in short can be found on erowid. If you can help me to identify what this crystals are i would realy appriciate. I also keep a sample of 4mg per ml MeOH in the fridge. If you can recommend a good solvent mixture for mobile phase for thin film chromotography i would be very thankfull. My attempts could not split the components.

These are pictures of the crystals i mean. First in Ethanol. Many Diffrent things, i always thougt only the clean smooth on the top are the correct ones. Is that correct? Picture 2 is also Ethanol. Picture 3. is Hexan, it is not the winter wonderland i expected. The crystals are dull and not pure white. The two images are petrol ether from base. Also these needles doesn't look right to me.

 

[Osmosis Vanderwaal]

I'm just some ahole on the internet, but here's my interpretation:
MARQUIS, no positive reaction
MORRIS, positive cocaine
ROBODOPE, no positive reaction
SIMONS positive cocaine
EHRLICH no positive reaction
MECKE, positive phenecitin
LIEBERMAN positive cocaine

The crystals. I am analyzing now I agree that pic 1, between 11 and 2vo'clock are the quintessential cocaine hydrochloride crystals I see
Pic 2 shows the same structure I see in my crystallayions that I believe is an analgesic "caine" benzocaine perhaps
Pic 3 is some beautiful cocaine crystals that seem mighty pure to me
Pic 4&5 have a monoclinic structure whose aspect and ratio match the literature for phenacetin

 

[Osmosis Vanderwaal]

In the first pic you can see that same structure I'm calling benzocaine. This is just solvated in ice cold RO drinking water@2ml/g, and quickly decanted into a pie pan and evaporated

 

[Osmosis Vanderwaal]

My wife was on my ass to do something other than look at cocaine crystals when I responded innitially, what I didn't get to say is, nice job on the reagent reactions and crystal photos, when I first responded I thought I was responding to some kid who was playing with his food, and you impressed me with the thoroughness of your response. I think we are in a similar place with similar motivations about cocaine. It's my favorite drug and I ve searched high and low for more information. I've found a ton but a lot of it is beyond the scope of my chemistry abilities.
There are secrets that remain hidden about this chemical and I hope to uncover them and I'll take all of the help I can get. Feel free to share any knowledge you uncover and I will also share mine with you. The latest find under the cocaine chemistry headline for me is the book, "the cocaine handbook" and "the cocaine users handbook " by David Lee. They are older publications (78 and 80) but contain a few bits of knowledge I didn't prevyliously know. They are available to download free from multiple places. If you haven't read them, you should. If you don't find them easily I can link you to the pdf download pages. I tried to upload one, but gave up after it failed 3 times.
I read that yellowish coloration isnt a positive reaction for Ehrlich and also is fairly common. I don't personally see green in it. Greenish yellow perhaps, which isn't concusmm×

 

[DanTheMan]

Wow, thanks for the friendly and respectful response. I'm sure we can find better ways to purify. Was the water recrystalisation that you meaned with "I can give you a scheme that will actually leave practically no trace of adulterant, " ? If I look in my notebook i tried it already 6 times never with success What i did:
-Fill 2ml water in testtube with screw lid
-put on screw lid and put in ice water
-meanwhile crush 1g material
-take testtube open it, and put poweder in it. (Maybe i was to slow here and the 2ml of water got room temp again)
-close testtube and shake -> very litlle is not dissolved
-pour from testtube leaning on glass stierer to avoid dripping and hold not dissvolded material back
-I used a glass cutting bords for this made out of tempered glass
-placed board on heating mat for terrarium (will never exceed 35°C) + used portable fan to help evap of water.
..... That took ages because the consistency was like maple sirup... i skewed the plate the get a bigger surface for heat and fan but still, very slow evaporation compared with ethanol. As soon it was no longer runny on my board i put it the a coold place near the windows so could wind will help crystalisation. And gues what? All the strange crystals a still here... + the no good effect anymore. The water and temp must hydrolized the sensible molecule... Next time i will put the cocaine also already in testtube in cold area, only add cold water, shake shortly and throw it porcelain buchner funnel with vacuum(I'm still unsure if vacuum actually can speed up hydrolysis,). To answer your question: Are you checking your ph as you do all this sciencing? Yes via well calibrated digital ph meter and normal test striped. Do you adjust the ph of your water to avoid this?
Like here https://drugs-forum.com/data/attach..._stability_of_cocaine_in_aqueous_solution.pdf
a ph value of 5 is recommended for room temperature storing.
Also of ofcourse i know the books from David Lee, it was also my starting point but now kinda outdatet....

 

[DanTheMan]

Can you explain how does soubility work ? I can find sources stating 2.7 - 3.2 ml ethanol can dissolve one gram. If i try with up to 4 ml per g. The stuff remaining in filter still tests positiv with morris reagent. My theory is there is some kind of sugar mixed in. The sugar can dissolve in water and forms goo, this goo can dissolve more cocaine? I'm pretty sure i already seen this with chloroform. If i tried the chlorform crystalisation without aceton wash and everthing got dissolved. But if the powder was correctly washed via aceton, i can filter out cuts with chloroform becuse not everything got dissolved. I think my enemy is an emulgator that helps thats diffrent compounds mix evenly.

 

[Osmosis Vanderwaal]

When you said it was sticky after it's bath. I knew we were talking about sugar. Mannitol probably , it's a sugar alcohol so it dissolves in ethanol methanol and water. I accidentally used NOT cold water once and it turned to brown glue and 20 extractions later i successfully lost all the cocaine. No, the decant, I usually do that exactly 1 time and if If I get something worthwhile out, I'll do the whole bag but 4/5 times I don't get anything. Boiling hot isopropyl does a pretty fair extraction for me most of the time. I put it in the Buchner, dump the hot iso on it swirl it for 5 seconds and hit the switch. Then I splash a few ml of boiling hot isopropyl to suck out the residual anything in the buchner.
If you take that ice cold water and neutralize it with some sb, you can pick the pebbles out and you have eliminated most if that sugar it stays dissolved in the water, then crush it, recook it in new water and a bit of base and collect it a second time. Did you know that c.hcl is so polar that it dissociates 50% in 7 ph water, using a ph meter is important because if your ph matches your pka, then technically it's 50% unionized and your in danger of losing 1/2 your shit. Make sure that you check that your ph is 2 past the pka at least but cocaine is also fragile and it breaks down easily. Acid extraction, ph<6.6 when you are trying to clean it, before you seperate the polar/non-polar, check the ph and adjust it because if it's 7 you are losing product. I've seen a few papers that addressed the presence of levamisole. There are 2 similar papers ( the second is a forgery and theft of intellectual property in my opinion). Both papers have 3 strength mixture samples of cocaine and levamisole and in both papers the successfully remove the levimisole via neutralizing it and cleaning it with hexane and then re-protonating it with hcl gas. The first paper I read though, although it heralded the Lewis acid reconjugation and 3x hexane wash as the featured route, cleaning all of the levamisole out in only 2 washes, if you read the paper, the other method also removed all of the Levamisole, but took 3 washes. It was chloroform on the hcl in water. Cocaine hcl dissolved in water, shaken with chloroform 3 times, then evaporated under vacuum. As I'm sure you know, Levamisole is the gold standard of hard to remove .
I've seen no evidence suggesting a course ( or strong for that matter) vacuum has any detrimental effect on cocaine. Which brings me to something I've never heard of or seen tried. Centrifuging. I was just hunting down the physical properties of mannitol and cocaine hcl and I noticed some interesting facts. Cocaine hcl has a mol. Wt. Of right at 2x mannitol. At the same time, mannatol has a polar surface area of 2x that of cocaine hcl ( more than, (120A vs. 55A) which makes it an amazing candidate for centrufuging. It's parachutes and torpedoes. Also 120 angstrom could be filtered out with a cellulose disk and you should be able to find a proper size one more than 55 and less than 120

 

[DanTheMan]

Since i own a centrifuge(or build one out of old drone motor) i'll give it a try.
To come back to the actuall topic and Answer my own question. Yes, cocain can be reoxidized for purification. See https://www.emcdda.europa.eu/publications/eu-drug-markets/cocaine/production_en#figure1

Just another link for the intrested. I think it's worth a read.

TEK - Removing adulterants from cocaine hcl for the real connoisseur

WARNING: A LOT OF THIS INFORMATION IS OUTDATED. ESPECIALLY THE HCL PART NEEDS A REWORK BECAUSE THE RESULTS ARE NOT PLEASING. ALSO THE NHEXAN PART WORKS...

drugs-forum.com

 

[Osmosis Vanderwaal]

YIKES! Is my initial impression of that second link. I don't suggest anything it says. I might but I would have to analyze it with factual information and run the numbers. My initial impression is it's a great way to lose a lot of product. I stopped reading it when I got to the 10th piece of false/ misleading information. It'll be a long journey to debunk all of that with citations.