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Cannabidiol (CBD) Isomerization to Psychoactive Cannabinoids

thcman

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Could someone please send some simple steps i have tried to extract with distilled water and syringe but when adding alcohol to the oil it turned purple?
 

Uncle Lee

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Turning purple means that your product contains a high percentage of CBD and that your ethanol solution is mixed with alkaline substances
 

Uncle Lee

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Why don't you try the citric acid isomerization method I posted in this forum, this reagent is easily available worldwide.
If you need a slightly larger scale or industrial scale production you can contact me and I can help you design it for a fee, but it requires some special reagents.
Any other questions you can leave a message and I will help you for free
 

Montecristo

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Isomerization of CBD to THC using citric acid

Please be safe, at least pretend you are a professional chemist when doing the experiment, wear glasses and gloves, and have a fire extinguisher handy

It is important to note that this process is designed to use readily available materials and reagents and to convert CBD to THC as efficiently as possible, both in terms of yield and time efficiency, and is not comparable to professional laboratory techniques.

Reagents.
Citric acid
CBD
Distilled water
Sodium bicarbonate or sodium carbonate
Non-polar solvent

Equipment:
Small flask (do not fill a boiling flask more than half full)
small leibig condenser (200mm will be fine)
Small pump for condenser, aquarium pump can be
Small tube to fit the condenser fitting
Small bucket to put the pump into
Heat source suitable for your flask, preferably a heating jacket with magnetic stirring
PH test strips
A scale accurate to the gram
Dispensing funnel


Isomerization.

Determine your batch size and then determine how much water you want to use. You can go as low as 1gr H2O:1gr CBD, but you can also use more water to make the mechanics a little easier. For 1g batches I usually use 5g of water, for 5g batches I usually use 10g of water.

Add the desired amount of distilled water to the boiling flask using a small stirring bar. To do this, add at least 15% by weight of water to anhydrous citric acid, food grade. (So 1g of water will contain 0.15g of citric acid, it does not matter how much CBD you use). Attach the reflux condenser to the flask and secure it with metal clips and tube clamps. Fill the condenser and leave the aquarium pump running continuously. Turn on stirring to ~75 rpm, heat to ~120C, and bring the solution to a boil. Reflux for anywhere from 4 to 12 hours, depending on the CBD/D8/D9 mix you want. The longer the reaction runs, the more D8 you get and the less D9 you get. I prefer about 8 hours. You can run small batch tests to see what reflow times will yield the product you like. If you want 100% D8, run the reaction for 10-12 hours or until the test is negative.

Post-treatment.

Neutralization: Once the allotted time is up, turn off the heat source and allow the solution to cool to room temperature. Remember, your target is insoluble in water and is a solid at room temperature. After cooling, your flask should have large chunks of solid product floating on top of the water and clumped against the flask walls. You neutralize the citric acid with some sodium bicarbonate (3 moles of sodium bicarbonate to 1 mole of citric acid). You can add the bicarbonate directly to your solution and test the pH, or prepare a concentrated bicarbonate solution and add it to your flask, it makes little difference. Test with pH paper to confirm ~7 pH (does not need to be exact, 6-8 is fine).

Extraction.

Next, in this flask, add a portion of NPS. you will need to experiment to see exactly the smallest amount you can use, but your target molecule is readily soluble in DCM or EtOAc at room temperature. for a 5 g batch, I usually use ~20-30 mL of DCM. spin the NPS and you will see that your product has dissolved. Separate the aqueous phase and discard (I do this in a separatory funnel). Wash the NPS with an equal amount of dH2O (20ml of NPS with 20ml of dH2O) to remove any impurities physically trapped/entrapped in the product. Re-separate. If the organic phase becomes cloudy, it has absorbed some water. Dry with MgSO4 until the solution is clarified again. Decant or filter to remove MgSO4.

Isolate the product.

Your product is now dissolved in the NPS. Ideally, you can extract and recycle this NPS, thus significantly reducing the cost and environmental impact. If this is not an option, you can simply heat your solution to allow the NPS to evaporate. Perform this operation in a well ventilated area
Uncle LeeFor NPS, can I use naptha without issue?
 

Uncle Lee

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Naphtha is not exactly the same from region to region, you need to test, this solvent evaporates without any residue and dissolves THC easily, then it is OK
 

Montecristo

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Naphtha is not exactly the same from region to region, you need to test, this solvent evaporates without any residue and dissolves THC easily, then it is OK
Uncle LeeOkay thank you, its the nap i use for DMT extractions and from that I know that it dries without residue but not sure about THC solubility. I could distill the DCM out of some paint stripper though, so I might do that first and then compare with with nap. Or I could try with nap first to see if it dissolves the THC, and have DCM on hand if it doesn't. Id rather use nap if possible due to it being cheap and accessible, I can update when i try this and let everyone know how it turns out comparatively .
When you speak of recycling the NPS, you mean via distillation ? if so, how would you recommend getting the product out of the boiling flask?
thanks!! I'm very excited to try this!!
 

Uncle Lee

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I prefer to use low boiling point solvents, if you do not want to recycle just water bath the solution directly in the outdoor evaporation, you need to recover the solvent then just distillation, if you are a home laboratory, you can pour the solution out into a flat bottom container when a small amount of solvent remains, water bath and evaporate the solvent, if you make large quantities, you can private message me
 

thcman

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Is isopropyl alcohol viable, what are the best solvents other than ethanol
 

thcman

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Should I leave Stiring when adding
Bicarb and water and how long should I leave to neutralise
 

Uncle Lee

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Isopropyl alcohol should be fine, but you want to make sure no isopropyl alcohol is left in your product. I rarely try to use ethanol as a solvent, I'm not familiar with that approach

You need to stir, the reaction will be gaseous in the presence of acid, the neutralization is very fast and you don't need to wait long
 

thcman

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Is it safe to boil off the acid, it looks good on the video are their any bi products for
Rom this and does it effect the isomerisation
 

Uncle Lee

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Without trying to boil out the acid, you can absolutely use a base and then extract with NP, wash, dry, and evaporate the solvent to obtain THC, which is very simple to do, just try
 

thcman

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Is hexane viable what is the safest option i like ethanol ol as seems safe and has no toxicity so you know any route with just ethanol
 

thcman

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Hexane would dilute with ethanol and thc to be extra sure its all boiled off, do you know of any websites with videos this is quite a common thing there alot of patents and recipes o google but I can't find d any with ethanol or hexane, do you know how to purify thc and re isomer cbd I have had some insights but reagents are toxic
 

thcman

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The video i saw isn't on here anymore is it safe to boil off acetic acid, should be getting np hexane soon I want some more research on toxicity before I do that what temperature should It evaporate off at
 

Uncle Lee

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It is theoretically safe for smoking, in fact I don't know what by-products are produced by boiling the solvent, perhaps acetate or acetyl products
If you have enough time you can let the solution evaporate until only the paste THC and a small amount of liquid remains, then extract with hexane, wash the organic phase with sodium bicarbonate solution, wash the organic phase with distilled water, dry the organic phase with anhydrous sodium sulphate and evaporate the solvent to obtain THC
 

thcman

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I do understand that way I don't have non polar ,hexane yet I am trying to make e liquid what should the product smell and taste like and are their ways to test for negative byproducts, is acetate dangerous valine or smoking its not vitamine e acetate what would make this product dangerous
 

WillD

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I do understand that way I don't have non polar ,hexane yet I am trying to make e liquid what should the product smell and taste like and are their ways to test for negative byproducts, is acetate dangerous valine or smoking its not vitamine e acetate what would make this product dangerous
thcmanFor the perfect can be used HCl aq. soln.
 

JoeShit

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I'm using bulk CBD and I don't think it's been winterized. When I ad baking soda to neutralize the acid it looks like all the fats and lipids crash out creating a very light and solid layer on the bottom, leaving alot of blackish liquid on top. I had desolved it in isopropyl alcahol from the beginning, so now I have the black liquid in a large plate to let the alcohol evaporate.
 
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