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Caffeine freebase extraction Options
 
۩
#1 Posted : 2/26/2013 1:12:57 AM

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How would you perform a caffeine freebase extraction and recrystallization?

Have a good one kungpow
 

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a1pha
#2 Posted : 2/26/2013 1:28:13 AM


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Doesn't help you much, but I buy mine online and it's great. Amazon has a great price for pharma grade powder, too. Probably cheaper than trying to extract.

http://www.amazon.com/Ca...-5&keywords=caffeine
"Facts do not cease to exist because they are ignored." -A.Huxley
 
۩
#3 Posted : 2/26/2013 1:38:00 AM

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Any idea what form the chemical is in and % of purity?
 
proto-pax
#4 Posted : 2/26/2013 3:29:59 AM

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oral bioviability of caffeine is greater than any other ROA, rate of absorption would probably be faster, but I have my doubts if this would produce any rush more of a significant rush than eating it. caffeine doesn't work like meth or cocaine feel free to try it though.
blooooooOOOOOooP fzzzzzzhm KAPOW!
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۩
#5 Posted : 2/26/2013 3:41:22 AM

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Good to know. I have an idea and need to experiment. I just need to understand the basics of producing the freebase form and purifying it so I can test.
 
Kash
#6 Posted : 2/26/2013 5:32:59 AM

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I'd imagine if it comes in salt form then you can just freebase it in aqueous solution with some ammonia or maybe even sodium bicarb. Then you could pull it from water layer into some chloroform or toluene and evap. That would be a good first route to try.
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
۩
#7 Posted : 2/26/2013 5:37:02 AM

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Thanks. Some procesures use EToH to re-x but this is for the salt forms.
I'm assuming this is not the case with freebase and something like toulene would be better?
Are there any alternatives to toulene and chloroform?
 
Kash
#8 Posted : 2/26/2013 5:43:59 AM

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Possible alternatives would be xylene, d-limo, maybe even naptha. I would think that since the freebase should be insoluble in water, that it could be recrystallized in acetone/water or acetone/ethanol. This is all speculative though. Sounds like a fun little experiement. Smile
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
۩
#9 Posted : 2/26/2013 5:47:01 AM

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Quite fun indeed...
Would you do the acetone and water mixture at 1:1?
 
Kash
#10 Posted : 2/26/2013 6:03:23 AM

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No, I would cover the freebase with water and heat it with stirring, then add acetone until it all dissolves. If you hit close to the saturation point while hot, then crystals should precip with cooling if all goes well.
--------------------------------------------------*Kash's LSA Extraction* * Kash's Mescaline Extraction*------------------------------------------------------
All things I say are complete and utter ramblings of nonsense. Do not consider taking anything iterated from the depths of my subconsciousness rationally and/or seriously.
 
Mindlusion
#11 Posted : 2/26/2013 7:13:42 AM

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I'm extremely glad you posted this ۩.

Caffeine is very cheap online, like a1pha mentioned, but where's the fun in that? Besides, coffee tastes better.

I've extracted caffeine from roasted beans, using a simple A/B extraction.

Basically, I made a strong, righteous brew. Defatted with DCM, Basified with NaCO3, and pulled with dcm.

The crude extract was purified with a sublimation technique. Very effective with caffeine because it will not decompose at boiling temperatures, the resulting crystals were scrapped off the condenser and were weighed.

I got an extremely small yield, something like 300mg for 100g of coffee. (Likely do to loses in the de-fat and due to its solublity it water.)

The substance was similar in activity to the caffeine freebase I bought online.

Xanthines > ftw

^
ya hear?


---

Caffeine doesn't make salts like the amine alkaloids do.(Just take a peak at its pKa....)
( You do NOT want to dose caffeine HCl) The freebase is very stable.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
۩
#12 Posted : 2/26/2013 7:18:16 AM

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So you're saying caffeine is always a freebase?
Even the USP grade stuff?
 
Mindlusion
#13 Posted : 2/26/2013 7:27:46 AM

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Kash wrote:
Possible alternatives would be xylene, d-limo, maybe even naptha. I would think that since the freebase should be insoluble in water, that it could be recrystallized in acetone/water or acetone/ethanol. This is all speculative though. Sounds like a fun little experiement. Smile


caffeine freebase is totally soluble in water.

Especially hot water, it is extremely soluble in hot water.


Do you have any idea how acidic and unstable the hydrate salt would be?


Solubility of freebase caffeine can be increased with the addition of a hydrotrope. like an alkali salt. ( Sodium citrate, or sodium fumarate) Thanks to the ionic interactions...


If you want to migrate freebase caffeine over from a basic solution, it better if its ice cold...



You can very easily recrystallize caffeine by supersaturating it with water...


It's solubility at boiling temps is magnitudes greater, I had problems with it precipitating too fast! Grew extremely fine crystals that resembled cotton fibres.

---
Sort of, house. The salts do exist. But its unlikely you'll ever run into them.

HCl for one is incredibly unstable. USP grade is labelled citrate. I believe it is a combination of freebase and sodium citrate. bear in mind, they are not salts if they are still dissolved solution, merely ions.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Mindlusion
#14 Posted : 2/26/2013 7:32:57 AM

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oral is by far, the best ROA of caffeine. and it is best administered dissolved in warm water infused with coffee bean oils.


Believe me. Out of curiosity I tried practically all the ROAs you could think of Razz

---

Besides, dosing a pure powder will jack up your tolerance, just like any drug.
I prefer the crude waterbased extract

Doing cocaine is going to cause more trouble then drinking coca tea.

Same deal here with coffee. Except we are dealing with caffeine. Obviously.

Or drinking a shot of bourbon, compared to a glass of beer
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
۩
#15 Posted : 2/26/2013 8:44:40 AM

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So you're saying you did a BUTTer shot of mxe and caffeine freebase before writing this very helpful information? <3
 
Jin
#16 Posted : 2/26/2013 11:21:12 AM

yes


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Stop

caffiene can be really dangerous , i've not posted this before however once i had ingested about 10 cups of coffee , all at the same time , ppls dont judge me i just wanted to get high , stupid and totally immature , i was young

what i had done was put 10 spoonfulls of coffee in a mug , added water and gulped it straight , i did'ne vomit or anything (i should have but could not ), was awake and terrified for 3 days straight , and am mentally yet to recover fully , it has been years

i tell this tale now , just for the sake of harm reduction and caution since messin with caffiene is extremely uncool , i have done some stupid things in my life and this was perhaps the topmost mistake

i don't want anyone to suffer that much , please be careful consuming caffiene , i dont know why you want to freebase caffiene ۩ , however i hope you tread with caution knowing caffiene overdosing can result in severe damages(psychological) , and i really don't know if freebase caffiene will have the same effect , however pls be careful with doseages , caffiene is not fun

i tell this tale now only for caution , i admit i have been very stupid , i would'nt have mentioned this however reading this thread i cannot let my fellow Nexian go down the same road if he intends too , pls i respect you alot ۩ , this tale is only so you know the dangers and don't overdose on it or something pls be careful

much respect
Jin

it was'nt even 10 spoonfullsi i hardly remember , the coffee Box was coming to an end i took 6 spoonfulls out of it and poured whatever was left in the Box into the mug(i had a very macho attutude at that point ), could have been only 8 spoonfulls , however i mention the morale of the story is not to mess with caffiene , i mention 8 spoon fulls now to let you know one does not need to go very high with doseage to be messed up with this substance 6-8 spoonfulls all at the same time can result is some very nasty changes to the psyche which might never heal , everyday gets better however no full recovery has yet been made , perhaps i should have vomited ........huhSad
illusions !, there are no illusions
there is only that which is the truth
 
Mindlusion
#17 Posted : 2/26/2013 3:23:03 PM

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۩ wrote:
So you're saying you did a BUTTer shot of mxe and caffeine freebase before writing this very helpful information? <3


well, Butt of course! Pleased

--


Jin, coffee connoisseurs like house and myself, we have developed a mutual bond, so to speak with the caffeine containing coffee beans.

and NO, its not about the dose, its about that first sip and that instant gratification.
This is where the real high comes from. IMHO its better then cocaine

xanthines > all drugs

Probably a good idea to put that out there, considering there are people out there that were once like yourself when you were young. Taking massive doses of caffeine will NOT get you high.


I can think of one time, I got my new dual action, low rpm concial burr coffee bean grinder, with 14 different grind settings.
I was tinkering with the settings on both my grinder and espresso machine, in hopes of creating the perfect cup, before I knew it, i had consumed 6 double espressos in about 20 minutes.

I experienced anxiety, and what I would say felt like a mild form of amphetamine psychosis. I also experienced peripheral hallucinations. I had heard about caffeine hallucinations, so I thought this part was kind of cool. Basically just white dots moving on my peripheries. No more visually fascinating then an eye floaty.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
benzyme
#18 Posted : 2/26/2013 3:38:15 PM

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basify to pH 9 with ammonia, extract with DCM, evap. (this will give colored crystals)
re-x with hot acetone. (this will yield white crystals)
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Infundibulum
#19 Posted : 2/26/2013 3:58:11 PM

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Mindlusion wrote:
I can think of one time, I got my new dual action, low rpm concial burr coffee bean grinder, with 14 different grind settings.
I was tinkering with the settings on both my grinder and espresso machine, in hopes of creating the perfect cup, before I knew it, i had consumed 6 double espressos in about 20 minutes.

I experienced anxiety, and what I would say felt like a mild form of amphetamine psychosis. I also experienced peripheral hallucinations. I had heard about caffeine hallucinations, so I thought this part was kind of cool. Basically just white dots moving on my peripheries. No more visually fascinating then an eye floaty.

For some reason, this excerpt reads like porno! You must truly love caffeine. Smile 6 double espressos amount to close to a gram of caffeine!

I am not a huge fan of coffee, but I do enjoy the odd double/triple espresso once in a while, strictly without milk or sugar, and it has to be some good stuff too. I used to be hugely in favour of maté, but I stopped it due to the huge amount of caffeine you take if you drink it the traditional way; it was making me feel washed out halfway during the day, which is a no-no.

I also used to snort caffeine as a student and found it to be just the right thing for these next-day deadline assignments. I have been also experimented extracting caffeine from green tea, particularly gunpowder green tea. I was slowly evaporating just-water tea extracts and I could see crystals after full evaporation. Green tea can easily have a 5% caffeine.




Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
jamie
#20 Posted : 2/26/2013 6:20:30 PM

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"Taking massive doses of caffeine does NOT do anything."

Huh? I have seen a person OD on caffine before, shaking and vomiting. It certainly does do something when you take a massive dose and caffine is linked to anxiety disorders etc..you can love it as much as you want but it is not a chemical lacking dangers when it is abused.

Drinking too much coffee is one of the most unpleasant experiences for me, and chronix use of the stuff just makes me feel spun out and then completely burnt..and it's horribly addictive when you try to quit after years of daily use. I drank a thermous a black coffee a day at one point, and while I really love coffee I had to quit for the above reasons and the headaches when one tries to quit are pretty bad. I wont drink it daily any longer just because of how hard it was to stop.
Long live the unwoke.
 
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