Cannabidiol (CBD) Isomerization to Psychoactive Cannabinoids

MuricanSpirit

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@William Dampier I appreciate your insights very much. Thank you again. You are doing hero work here. We should create own nobel prizes for the darknet because you are clearly helping humanity here.

Does anyone know a way how to make CBD solvable in water (if that's even possible)? I found on YouTube shops selling water solvable CBD and I'm suspect it's somehow "a trick" with the solution the CBD is in but how are they doing it?

I'm asking because pure "drinkable" Ethanol costs a lot here because of tax reasons (Alcohol to drink is heavy taxed so they tax Ethanol as well to avoid people buying it to create their own "moonshines"). Maybe I could use Methanol? I guess I could use some oil like Toluene as well (?) but I was thinking that it might be just cheaper to use distillated water instead (in which CBD doesn't solve well enough resulting in trapped CBD within its own oil not touching the solution. Sadly I have no stir bar hot plate, I have a hot plate and stir bar but they are separate units).

I'm sorry if I'm asking noob questions: I just recently started to be interested in chemistry and wish I would have studied it instead of what I'm doing now.
 
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Rabidreject

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@William Dampier I appreciate your insights very much. Thank you again. You are doing hero work here. We should create own nobel prizes for the darknet because you are clearly helping humanity here.

Does anyone know a way how to make CBD solvable in water (if that's even possible)? I found on YouTube shops selling water solvable CBD and I'm suspect it's somehow "a trick" with the solution the CBD is in but how are they doing it?

I'm asking because pure "drinkable" Ethanol costs a lot here because of tax reasons (Alcohol to drink is heavy taxed so they tax Ethanol as well to avoid people buying it to create their own "moonshines"). Maybe I could use Methanol? I guess I could use some oil like Toluene as well (?) but I was thinking that it might be just cheaper to use distillated water instead (in which CBD doesn't solve well enough resulting in trapped CBD within its own oil not touching the solution. Sadly I have no stir bar hot plate, I have a hot plate and stir bar but they are separate units).

I'm sorry if I'm asking noob questions: I just recently started to be interested in chemistry and wish I would have studied it instead of what I'm doing now.
MuricanSpiritYou should check out the book written by ‘Michael Valentine Smith’ a pseudonym of another well known psychedelic chemist and just a fantastic all round chemist, called Psychedelic chemistry. It was written, I believe, back in the 70’s. It has quite a bit about cannabis chemistry also…this stuff is not new, neither are the anologues that MAINLY were made by the US government.
it’s funny because movies like Pineapple Express make it seem like the US government developed the strongest weed in the world.
why would they bother when they had chemists working on D9-THCO! Remember most of the Thco that’s being sold all over the gaff is d8-thco which is quite a bit weaker IME.
it’s a good book to have although, I’m sure (well, I know) things have moved on a fair bit with regards some of the synths - it’s like pihkal is now obviously outdated in terms of available precursors - for the most part.
I think a lot of people see that it’s ’just Boiling CBD in an acid - any acid and you get 100% d9-THC - I’m not saying you, but iv seen idiots on Reddit asking about it with 0 analytical equipment - that’s the thing that scares me about working thing any cannabinoids - they are so sticky and generally annoying! I def have thought about doing this myself and then thought better of it when I realised there is no way to check what you have unless you are connected to a uni, basically.
Hamilton has a great podcast with him by the way, some really interesting stuff comes up durin the 2h discussion.
 

Uncle Lee

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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
 

Dr.Chocolate

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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 LeeHow long would I need to reflux to get d9 if Im using Sulfuric acid and ethanol?
 

Roberto Cofresí

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How can we combine these 2 patents ? To get high yield , high purity THC from CBD
 

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csigger

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The production of cannabidiphorol (CBDP) from CBD involves decarboxylation, where CBD is heated at high temperature (around 130-150 °C) to remove the carboxyl group, resulting in CBDA. The CBDA is then converted to CBDP through hydroxylation, using enzymes such as peroxidase.

A process involves the following steps:

  1. Preparation of necessary materials: CBD, hydrogen peroxide, peroxidase enzyme, ethanol, hydroxylamine, and other reactive materials.
  2. Decarboxylation: CBD is heated at high temperature (around 130-150 °C) to remove the carboxyl group, resulting in CBDA.
  3. Hydroxylation: CBDA is treated with hydroxylamine and hydrogen peroxide, and then mixed with peroxidase enzyme, which catalyzes the hydroxylation reaction to convert CBDA to CBDP.
 

csigger

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Ingredients:

10 g CBD (cannabidiol) powder
50 ml ethanol
1 ml peroxidase enzyme solution
50 ml 30% hydrogen peroxide solution 50 ml acidic water (pH 4)

Equipment:

Test tube
Thermometer
Agitator
Pipette

Preparations:

Prepare all equipment and materials. Clean and sterilize the equipment.

Steps:

Weigh 10 g of CBD powder and add it to a test tube.Add 50 ml of ethanol to the test tube.Add 1 ml of peroxidase enzyme solution to the test tube.Mix the contents of the test tube thoroughly with an agitator.Add 50 ml of 30% hydrogen peroxide solution to the test tube slowly while stirring.Monitor the temperature of the mixture with a thermometer, making sure it stays between 20-30°C.Allow the mixture to react for 2 hours, stirring occasionally.Add 50 ml of acidic water (pH 4) to the test tube and mix well.Extract the resulting mixture with a pipette and transfer it to a separating funnel.Allow the mixture to separate into two layers, with the top layer being the kannabidiphorol.Carefully drain the top layer into a clean container and discard the bottom layer.
 

Ecko6ap

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Ingredients:

10 g CBD (cannabidiol) powder
50 ml ethanol
1 ml peroxidase enzyme solution
50 ml 30% hydrogen peroxide solution 50 ml acidic water (pH 4)

Equipment:

Test tube
Thermometer
Agitator
Pipette

Preparations:

Prepare all equipment and materials. Clean and sterilize the equipment.

Steps:

Weigh 10 g of CBD powder and add it to a test tube.Add 50 ml of ethanol to the test tube.Add 1 ml of peroxidase enzyme solution to the test tube.Mix the contents of the test tube thoroughly with an agitator.Add 50 ml of 30% hydrogen peroxide solution to the test tube slowly while stirring.Monitor the temperature of the mixture with a thermometer, making sure it stays between 20-30°C.Allow the mixture to react for 2 hours, stirring occasionally.Add 50 ml of acidic water (pH 4) to the test tube and mix well.Extract the resulting mixture with a pipette and transfer it to a separating funnel.Allow the mixture to separate into two layers, with the top layer being the kannabidiphorol.Carefully drain the top layer into a clean container and discard the bottom layer.
csigger1. Will ipad work instead of ethanol?
2. Peroxidase solution is needed in what concentration? there are 150 units per milligram, there are 250 units per milligram.
3.does the cbd isolate powder need to be heated before this reaction? Because if you heat it up, it will melt.
 

Dr.Chocolate

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What does "10M" NaoH mean? How much is that? Also 2.80min and 3.40 min? I dont get it, can someone further explain?
 

T0lek511

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I dont know if it realy works
 

dbcooper

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I dont know if it realy works
T0lek511There is no way to make CBDP from CBD, you must synthesize CBDP from resorcinol and olivetol. It occurs naturally but only in extremely trace amounts.

Turning CBD into mixed THC's is incredibly easy. Just dissolve your CBD in alkane solvent (1:2 ratio, 100g CBD: 200ml Solvent), and add in a gram of pTSA (or a few drops HCl), and stir at room temp overnight. Wash the solvent with a few washes of 5% baking soda, a few washes of brine, than a few washes of pure water. Evap your solvent and than vacuum distill the remaining oil. (If you dont vacuum distill or do chromatography, than itll have more impurities).
 

dbcooper

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There is no way to make CBDP from CBD, you must synthesize CBDP from resorcinol and olivetol. It occurs naturally but only in extremely trace amounts.

Turning CBD into mixed THC's is incredibly easy. Just dissolve your CBD in alkane solvent (1:2 ratio, 100g CBD: 200ml Solvent), and add in a gram of pTSA (or a few drops HCl), and stir at room temp overnight. Wash the solvent with a few washes of 5% baking soda, a few washes of brine, than a few washes of pure water. Evap your solvent and than vacuum distill the remaining oil. (If you dont vacuum distill or do chromatography, than itll have more impurities).
dbcooperFor the solvent, pentane works as well as heptane. Hexane also works well but stay away from hexane since its more toxic.
 

LilianaHickman

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Interesting topic! It's crucial to understand CBD isomerization. If you're curious about safe and reputable CBD products, check out https://releaf.co.uk for more info. Knowledge is power when it comes to cannabinoids!
 

Irving Langmuir

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A long time ago, I tried isomerizing CBD to THC. This works well using 26% HCL as acid catalyst and 80% ethanol as solvent. Nevertheless, 24 hours of reflux were necessary.

Indeed, in my first test, with 8h of reflux, very little CBD was isomerized.

So, I'd advise anyone trying this reaction to periodically test their reaction medium: simply take a sample of your current reaction and put it in an aqueous solution of NaOH or KOH. If it turns purple, there's still a lot of CBD left.

In my case, it was only after 24 hours that the test did not turn purple.

At the end of 24 hours reflux, the ethanol had turned yellow, was evaporated, and an orange oil remained in the evaporating dish.

I've read from several sources that the longer the reflux time, the more delta 9 converts to delta 8, so you need to find a good reflux time so that the CBD isomerizes enough, but delta 9 doesn't fully convert to delta 8 unless that's what you want.

Moreover, the presence of water facilitates the conversion of delta 9 to delta 8 (apparently), so carrying out this reaction in an apolar solvent with an acid such as p-Toluenesulfonic acid would undoubtedly give a higher yield of delta 9.

Some people use aqueous hcl in an apolar solvent with strong agitation to mix the two immiscible solvents and apparently that works too.
 
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