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Cannabidiol (CBD) Isomerization to Psychoactive Cannabinoids

MuricanSpirit

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Do you have reflux condeser? Can you show the photo? Are there any flasks then?
William DampierRefulx = Returns the drops back the to heating solution? No I don't have those.

But I have 2 like this:
JQKSLAHJt3


And 2 with a spirale tube at the inside.


I don't have any flasks becaues I work only with jars. I'm thinking about renaming myself to Jarry.
 

HerrHaber

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Refulx = Returns the drops back the to heating solution? No I don't have those.

But I have 2 like this:
View attachment 2233

And 2 with a spirale tube at the inside.


I don't have any flasks becaues I work only with jars. I'm thinking about renaming myself to Jarry.
MuricanSpiritJarry, please try to addapt some rubber plug with hole inside to fit your condenser.
 

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
 

Ecko6ap

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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 Leeif we reflux for 4 hours, how much delta9 will we get?
 

edyf0101

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Hello all,
After reading this thread I decided to do the CBD Isomerisation using Citric acid.
I bought 100g of CBD Isolate 99% for 100 USD (I'm from Europe), Anhydrous Citric Acid and Etyhl Acetate and acquired a basic distillation set, soxhlet extractor and a heating stirring thing.
I used 10g of CBD.
I began doing it at 7pm. Getting CBD into the flat bottom flask was a challenge, the funnel got clogged and it solidified hard, minor wastage. Tips for other newbies, use a makeshift paper funnel.
~+20g of previously distilled water with 3g of Citric acid was also added and stirred till dissolved.
Refluxing showed a change almost immediately, with what looked like gold snot flowing in the water.
This grew over the course of a few hours. By the progress had slowed, I took a temp reading and it was at 100c, I turned it up a bit more but my heater has no measure of celcius on it and I only have a mercury thermometer so getting accurate and fast readings was not easy, as I had no access to the solution while it was refluxing.
By the 8 hour mark I took it off the heat and let it cool. It was 4am at this point and I fell asleep, it sat and solidified on the bottom overnight, it looked light gold when spread out.
I added 50g+ of ethyl acetate and it quickly dissolved, this was then put into a separatory funnel and I purposefully left some of the organic phase behind to avoid water contamination and have put it aside for further processing.
Distillation now began and was done in 2 hours, once there was a slither of my NPS left I poured it into the bottom of an aluminum soda can. I put a blower fan above and applied heating below, it may however have gotten very hot.
It quickly dried out and I was left with a dark amber puddle that was extremely sticky.
I do have pictures of the product but not of much else.


A few questions I would like answered by someone who knows.
1) How can I find out how much D9/D8 I made?
2) I heated the product during open air evaporation very high and I am unsure, what can happen if I bring this to a high temperature with my NPS and the open air for it to react to?
3) I want to perform another distillation at to seperate the unreacted CBD, D9 and D8 from one another. I have seen the temperatures it would take and I am worried that it will instantly cool in tube and I will be unable to get the product out. My only solution I can think of doing is:
a) Pull a vaccum to lower the boiling point.
b) Pump boiling hot water into my liebig condensor to help it flow through.
c) A combination of both.
4) I have been interested in using pTSA and Toluene to do a very pure reaction on a paper I saw. Where I live Toluene is becoming difficult to get in pure form due to its environmental hazards and pTSA would add an additional layer of complication. Is it even worth pursuing for a novice?


I hope you either were entertained or learned something from this post.
 

Latin King

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Hello all,
After reading this thread I decided to do the CBD Isomerisation using Citric acid.
I bought 100g of CBD Isolate 99% for 100 USD (I'm from Europe), Anhydrous Citric Acid and Etyhl Acetate and acquired a basic distillation set, soxhlet extractor and a heating stirring thing.
I used 10g of CBD.
I began doing it at 7pm. Getting CBD into the flat bottom flask was a challenge, the funnel got clogged and it solidified hard, minor wastage. Tips for other newbies, use a makeshift paper funnel.
~+20g of previously distilled water with 3g of Citric acid was also added and stirred till dissolved.
Refluxing showed a change almost immediately, with what looked like gold snot flowing in the water.
This grew over the course of a few hours. By the progress had slowed, I took a temp reading and it was at 100c, I turned it up a bit more but my heater has no measure of celcius on it and I only have a mercury thermometer so getting accurate and fast readings was not easy, as I had no access to the solution while it was refluxing.
By the 8 hour mark I took it off the heat and let it cool. It was 4am at this point and I fell asleep, it sat and solidified on the bottom overnight, it looked light gold when spread out.
I added 50g+ of ethyl acetate and it quickly dissolved, this was then put into a separatory funnel and I purposefully left some of the organic phase behind to avoid water contamination and have put it aside for further processing.
Distillation now began and was done in 2 hours, once there was a slither of my NPS left I poured it into the bottom of an aluminum soda can. I put a blower fan above and applied heating below, it may however have gotten very hot.
It quickly dried out and I was left with a dark amber puddle that was extremely sticky.
I do have pictures of the product but not of much else.


A few questions I would like answered by someone who knows.
1) How can I find out how much D9/D8 I made?
2) I heated the product during open air evaporation very high and I am unsure, what can happen if I bring this to a high temperature with my NPS and the open air for it to react to?
3) I want to perform another distillation at to seperate the unreacted CBD, D9 and D8 from one another. I have seen the temperatures it would take and I am worried that it will instantly cool in tube and I will be unable to get the product out. My only solution I can think of doing is:
a) Pull a vaccum to lower the boiling point.
b) Pump boiling hot water into my liebig condensor to help it flow through.
c) A combination of both.
4) I have been interested in using pTSA and Toluene to do a very pure reaction on a paper I saw. Where I live Toluene is becoming difficult to get in pure form due to its environmental hazards and pTSA would add an additional layer of complication. Is it even worth pursuing for a novice?


I hope you either were entertained or learned something from this post.
edyf01011. you need to get it lab tested. in europe that will be a problem because not many can dot it and labs dont allow you to ship them samples.
2. avoid high temp as much as you can some d9 wil turn to d8 or cbn.
3. you can only separate it with chromatography
4. not realy. people get good yield with heptane and hcl also with other easy to get stuff

@edy you need to neutralize the citric acid and rinse with baking soda and water. this wil also remove sodium citrate and salt created by neutralizing.

the wash can be done with hot water no nps needed. you can distil after that wihout nps also.

Also dont look at the reflux time. just make a beam test to see how much cbd has converted and stop when most is done
 

edyf0101

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1. you need to get it lab tested. in europe that will be a problem because not many can dot it and labs dont allow you to ship them samples.
2. avoid high temp as much as you can some d9 wil turn to d8 or cbn.
3. you can only separate it with chromatography
4. not realy. people get good yield with heptane and hcl also with other easy to get stuff

@edy you need to neutralize the citric acid and rinse with baking soda and water. this wil also remove sodium citrate and salt created by neutralizing.

the wash can be done with hot water no nps needed. you can distil after that wihout nps also.

Also dont look at the reflux time. just make a beam test to see how much cbd has converted and stop when most is done
Latin KingI did neutralise this sorry for not including that.
Thank you for your answers.
If I buy HCl I may as well get pTSA because both things you need to have a reason to buy them.
Basically any interesting chemical I have to synthesize myself.
 

Ecko6ap

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I did neutralise this sorry for not including that.
Thank you for your answers.
If I buy HCl I may as well get pTSA because both things you need to have a reason to buy them.
Basically any interesting chemical I have to synthesize myself.
edyf0101does it have psychoactive properties? how powerful is it?

how much distillate did you get from 10g of cbd?
 

blosuetoday

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Aproxximately how much psyhoactive substance can I get from 100g of CBD Isolate 99%?
 

edyf0101

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Aproxximately how much psyhoactive substance can I get from 100g of CBD Isolate 99%?
blosuetodayNot a chemist here.
Found this https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8011986/ CBD Isomerisation study on google. It has a few graphs regarding how much for a few of the different methods.
I've seen online but no studies saying that the Citric Acid in distilled water method at 120c for 8 hours, the easiest one for a newbie, will get you ~45% yield of D9THC, the kind most people want, however you also get roughly ~45% D8THC and some unreacted CBD. Read the whole thread, find which method you want, and look online for a source with a reading of amounts.
 

Latin King

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Aproxximately how much psyhoactive substance can I get from 100g of CBD Isolate 99%?
blosuetodaythe yield depends on the acid,nps and time. citric acid and zeolite are easy but have very low yield! with low i mean 50% or less,its horrible
 

aa1178251182

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Does CBD have to isomerize THC with 95% ethanol? Can I use 99.9% ethanol? What is the pH adjusted to with glacial acetic acid?How many hours does the reflux have the highest 9-THC yield?
 

HerrHaber

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Does CBD have to isomerize THC with 95% ethanol? Can I use 99.9% ethanol? What is the pH adjusted to with glacial acetic acid?How many hours does the reflux have the highest 9-THC yield?
aa1178251182absolute EtOH is obviously the best but consider expenses... it's worth it if you want to be an elegant chemist
 

weeds

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I want add THC to CBD weed. Is just do this?
1 - reflux 100g CBD isolate in ethanol and acid for 4-8 hours, using a method from this thread.
2 - with a syringe add the THC solution to about 200g? CBD flowers.
 
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