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Cannabidiol (CBD) isomerization to psychoactive cannabinoids

William Dampier

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With Battery acid:
1. 1 g of CBD was added to 35 ml of 95% ethanol in a 50 ml Round Bottom Flask (RBF).
2. Placed in a hot water bath at 70 *C.
3. Once the CBD was dissolved, 4 drops of 35% sulfuric acid were added to acidify the solution, pH < 3.
4. The mixture was allowed to reflux for 24 h in the water bath of 70 *C.
5. Once complete, 5 drops of 10M NaOH was used to basify the solution until the pH was greater than 10, which removes the sulfuric acid as sodium sulfate.
6. The reaction was then filtered to remove the sodium sulfate, which allowed for just the cannabinoids to be in the remaining ethanol solution.
7. The 0-h sample extraction resulted in only CBD being found at 2.80 min, which agrees with the reference samples of 2.80 min. After 1-h, the CBD peak was reduced, but still was the main peak present. However, other impurities began to increase after 24 h such as at 2.18 min and 3.40 min, which were found to be 8-OH-iso- HHC and 9α-OH-HHC. Additionally, the D 9-THC and D 8-THC doublet was found at 4.10 min and 4.22 min. Another peak at 3.77 min was found to be an isomerization peak of D 9-THC and is thought to be D 11-THC or D 7-THC. This method did not isomerize all the CBD even at 24 h. However, the CBD peak was no longer the most prominent peak in the sample. The largest peak was found to be the 3.38 peaks, which was 9α-OH-HHC.​
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With Muriatic acid:
1. 1 g of CBD was added to 35 ml of 95% ethanol in a 50 ml RBF.
2. Placed in a hot water bath at 70 *C.
3. Once the CBD was dissolved, 47.3 ml of 37% hydrochloric acid were added to the solution, making it a final concentration of 0.05% HCl with a pH of less than 5.
4. The mixture was allowed to reflux for 24 h in the water bath of 70 *C.
5. The 0-h sample extraction resulted in only CBD being found at 2.80 min, which agrees with the reference samples of 2.80 min. After 1-h, the CBD peak was reduced, but still was the main peak present. However, other impurities began to increase after 24 h such as at 2.18 min and 3.40 min, which were found to be 8-OH-iso- HHC and 9α-OH-HHC. Additionally, the D 9-THC and D 8-THC doublet was found at 4.10 min and 4.22 min. Another peak at 3.77 min was found to be an isomerization peak of D 9-THC and is thought to be D 11-THC or D 7-THC. Fragmentation was conducted and found that it has the same fragmentation and ratios as D 9-THC and D 8-THC, confirming that it is an isomer of D 9-THC and D 8-THC. This method did not isomerize all the CBD even at 24 h. However, the CBD peak was no longer the most prominent peak in the sample. The largest peak was found to be the 3.38 peaks, which was 9α-OH-HHC.​
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With Vinegar:
1. 1 g of CBD was added to 35 ml of 95% ethanol in a 50 ml RBF.
2. Placed in a hot water bath at 70 *C.
3. Once the CBD was dissolved, 1.909 ml of 99% glacial acetic acid were added to the solution, making it a final concentration of 5.2% acetic acid.
4. The mixture was allowed to reflux for 24 h in the water bath of 70 *C.
5. The 0-h sample extraction resulted in only CBD being found at 2.80 min, which agrees with the reference samples of 2.80. After 1-h, changes of CBD isomerization were only found as an increase in the peak at 3.77, which is thought to be D 11-THC or D 7-THC. After 4h, a noticeable peak of increasing D 9-THC was found to increase. At 24 h, the reaction was analyzed and found that 11-5 00 -dihydroxy-CBD, 8-OH-iso-HHC, CBD, 10-methoxy-THC, and D 9-THC were found at 1.96 min, 2.22 min, 2.80 min, 3.50 min, and 4.11 min, respectively. The compound at 3.77 min was found in these spectra and was the most abundant after 24 h.​
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MuricanSpirit

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Some questions regarding the vinegar method:

  1. Shouldn't it be possible to stop the reaction at any given time with soda? Eg. if I wish to get D9 I could add some soda after 4h reaction, right?
    1. Lets say I don't want any soda left over: Could I just evaporate the ethanol+vinegar to stop the reaction instead of using soda?
      1. It shouldn't make a difference if I increase the temperature that way that all ethanol+vinegar is evaporated after 5-6h?
  2. And isn't it possible to use 15% citric acid instead of 5% acetic acid which should return the same results?
    I just realized acetic acid makes more sense because it can be evaporated below CBDs melting point. I was afraid that it might affect the taste but it can probably be washed away and 2ml in 50ml ain't a strong smell.
  3. The amount of used CBD (as long as it dissolves well) isn't relevant eg. I could use 2g in the same 50ml solution, right?

Source
 
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William Dampier

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1. You can stop isomerization at any time by cooling the reaction. The boiling point of vinegar will not allow the idea of evaporation to be realized. With an increase in temperature, isomerization can proceed faster, but in a completely different way.
2. When using a saturated solution of sodium (or potassium) hydroxide, we get a dense aqueous layer from below, into which vinegar will go in the form of sodium acetate too. Above there will be a pure ethanol extract, which, after decanting, we can evaporate to obtain pure cannabinoids.
3. When scaling up, we can reduce the amounts of ethanol based on the actual solubility, that's right.
 

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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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William Dampier

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Water-soluble CBD is possible, it is obtained by creating complexes that change the original property, for example, with beta-cyclodextrins. This can be discussed in another topic, since these complexes are not suitable for the above isomerization process.

As for the use of methanol, toluene (benzene), it is possible, but the reaction conditions will be different. There is data on the isomerization of CBD in THC in benzene + PTSA and data on the use of methanol and hydrochloric acid, as well as methanol and PTSA. We can experiment with a variety of low boiling solvents and strong acids (acetic acid is relatively weak, but still suitable).
 

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Well I'm going to buy today hydrochloric acid (30%), ethanol 93% (or even 96%, don't remember), Toluene and Sodium hydroxide from pharmaceutical origin. I already have some food grade acetic acid.

And I have 300g CBD, the party can start! For legal reasons I can't produce more than 10g batches.

View attachment 2212

The quality seems to be good, according to the provided lab test (can be checked online a with QR code) it's above 99% but he could have cut it in the meantime so I decided to mix it with water (when I buy noids from China there are multiple layers of the powder eg. a part of the powder can reach the bottom while the other part flows above the water).:

View attachment 2214

After about 12h the CBD still doesn't solve with water:

View attachment 2213

Darknet Nobel Price candidate Dr. prof. William Dampier, tell me what to do and I will record it as video and share the knowledge.

Let's just "assume" I'm an idiot...

I have an industrial fan (made to remove the heat when growing cananbis). I'm pretty sure its enough (about 500L/s) because you can't really breath with that thing on.

Lab protection gear will arrive today:

  • Mask (replacable filters) with built in glasses (it looks like it will stick on your face)
  • Some cheap glasses (which don't give me a safe feeling)
  • Water resistant mask for skiing (to protect my skin on the head
  • Cotton lab jacket, looking for a chemical proofed which can be removed within seconds when needed
  • Nitrile gloves

I don't need this protection as long as I don't work with HCL, right? So I will train (gain lab protection experience) at the beginning with food safe methods like the vinegar method and move on to use HCL.
 
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William Dampier

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What you have, a pure material of the CBD, is great! The working area for chemistry should be as close as possible to the location of the exhaust fan. Collect the walls on the sides of the working area to increase the efficiency locally. Working with hydrochloric acid is not very dangerous if we use exhaust ventilation, gloves and caution. Take more subtle nitrile gloves for the convenience of work and change them more often in case of contamination. Thick gloves can create more problems than security. Using a full-face filter mask is a good idea anyway. In the role of protective clothing for work, quite approach DuPoint Tyvek. Such overalls or similar to them can be bought with a margin. Waterproof rubber boots will be the best solution to protect the feet. If hydrochloric acid got on the skin, rinsed with plentiful water with soap. If we have some skin reaction to acid, it would not be bad to have antihistamines at hand. If suddenly we strongly inspired a pair of hydrochloric acid, then we carry out the hyperventilation of the lungs. 15 minutes deeply inhale and exhale, quickly and frequently, outdoors. But in general, work with hydrochloric acid is not so dangerous as it seems. If you have valuable metal objects in the working area, I advise them to remove them, since there is a risk of corrosion from the vapor of acid. These are general recommendations, but regarding our particular case of hydrochloric acid in the reaction is not so much, to be worried about it.
 
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MuricanSpirit

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Thank you.

I guess the most noob friendly reaction is the "acetic acid reaction", right? I think for safety reasons until I have enough "training" I'm gonna use this one.

Does it have to be glacial, is it possible to use liquid acetic acid (room temperature)?

Lets say we are at the end of the reaction so we cool it down to stop it.

Now I'm left with THC in Ethanol mixed with acetic acid.

How do I remove the ethanol and acetic acid?

Will it work if I just let it freeze it down to 0° (normal freezer). Ethanol will still stay liquid but the acetic acid should become a solid at 8° so I can just pick it out, right?

If I want to remove the Ethanol can I just heat it up to 80° (preheated and as flat as possible to increase more contact between ethanol and hot air) to evaporate the ethanol?
 

William Dampier

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First, check the percentage of "household" acetic acid. You may need a little more ethanol to dissolve if the acid is too aqueous. Of course, we use liquid acid, in the case of chemically pure glacial acetic acid, it will freeze into crystals at 16*C, but we need warming up. Separating the acid after freezing is a bad idea, the alcohol will keep it in itself. We extinguish the remainder of the acid with a saturated solution of alkali, and it will go into a water-soluble metal salt. A dense saturated aqueous solution of salts and alkali will allow the mixture to separate into two layers, lower aqueous layer, and upper layer of ethanol extract with THC. By separating the ethanol layer, we can evaporate it.
 

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Thank you. So what akali should I use? I have sodium carbonate (and I will soon have sodium hydroxide), do you think those will work? And how much akali do I need per acetic acid? I have the feeling the answer might be not as simple as "3mg soda / 1ml accetic acid" so just throw me some lecture to me (links) I should read before I ask such dumb questions again.
 

William Dampier

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Sodium hydroxide would be u best bet. You can use a fairly concentrated solution of 1 g of alkali in 2 ml of water. It will take up to about 1.5 g of sodium hydroxide per gram of CBD.
 
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MuricanSpirit

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You were right, I had to buy some acetetic acid as well (98%)

This is what Ive done so far:
  1. Mixed 10g CBD in 50ml Ethanol (96%) (disolved very quickly). Used a small jar (plastic was only used when I had to measure the ml).
  2. Moved it into an preheated oven at 70° (air circulation was turned off.
  3. It took a while (about 50min) until the solution was 70° C (checked it with temp measurement wich are actually meant to check the temperatur of grill steaks etc).
  4. Added 2ml acetetic acid.
  5. Stayed for about 10h in the oven. Cooled down to roomtemperature since then.
I underestimated the smell. It ruined the oven. I think I got rid of the smell by just running the oven at 300° (pretty happy that it can clean itself).

Now I'm left with 23ml Ethanol. It still smells very bad - I don't smell any Ethanol anymore but only acetetic acid. If I remember it correctly it smelled more like Ethanol before the evaporation began. Did I do something wrong?

I wish there was a way to test it if it makes high...
 

William Dampier

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After adding acetic acid, it was necessary to measure the pH. Do not make a reaction in the oven, it is dangerous! Evaporations should go to exhaust ventilation. Very dangerous using the oven. We need a hotplate and stirrer ideally, indicator paper.
 

William Dampier

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If you are engaged in growing, then the acidity of the soil and mixture of fertilizers was controlled. You need a calibrated electronic pH-meter or pH-indicator paper. By adding any of the above acids, we focus more on pH < 3, That is, the indicator paper must be red, acidic. Then we can have the isomerization process when heated. For heating, it is better to use heat-resistant glass and a magnetic stirrer. Heating only under exhaust ventilation or with a cooling condenser. Ethanol evaporation can lead to ignition. The fire extinguisher at hand would be a good idea.
 
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William Dampier

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So... We use open air, no oven, microwave and similar in this case. For heating under exhaust, we use a hotplate or magnetic stirrer. When heated on the electric hotplate is stirring a glass or teflon stick. If we have a magnetic stirrer, in the kit there is a teflon magnet for stirring. In this case, for the reaction, we can use a flat-bottomed glass flask with a condenser.
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With reflux condenser without cooling evaporation will fly above, and safer. With condenser cooling, we can make a reaction, without cooling - evaporation of ethanol.
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Approximately, this should be indicator paper after the addition of acid to the reaction mixture.
Ethanol boils about 80 *C, we should not give it to evaporate completely ahead of time. Full evaporation of alcohol we can only admit after adding alkaline water and separating alcohol from the mixture. What you got like an unsuccessful experience, save for further action. Acetic smell should be removed when processing with an alkaline solution.
 
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MuricanSpirit

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Ok, I guess I was lucky then and or 27ml wasn't enough.

I will try to make myself a lab with cannabis grow equipment (Ive got a 1.2mx1.2mx2m tent and 1.2m round table and I guess they just add up perfectly. I can open it from one side completely and work basically from the outside. (I wouldn't stay in the tent) The fan will remove/pump the air out of the tent (in best case all tech eg. power adapters etc. are outside the tent).


What do you think is better to pump the air out of the tent (the fan is physically outside, tech gets less exposure of the inside). I will use a carbon filter at that tube which pumps (so the chemicals have first to enter the filter before they go through the fan pushed to the next tube which leads out to the outside).

The problem is the fan _could_ leak (shouldnt happen) so I guess for my safety it's better to put the fan into the tent and just protect it with some tape from contact to the chems (?).

Imagine it like this:

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But the fan would be outside. There would be no rotating fan in the inside (cornor). No big lamp. Those lamps have usually ropes which have can be set to different lengths (so you can control the distance to the polant). I would use those to control the distance to the evaporation.
Just imagine it with a table at the inside and 2m height.

Do you think its ok to have tech inside it?

Maybe we should move this comment here to "Tent home lab"?


P.S. We just posted at the same time. Yes I will buy a stirring hot plate.
 

William Dampier

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Yes, we can use the "chemical tent", "grow box" for our purposes. This is practiced frequently. A folding tourist table can become a working area in a tent. The following actions are trying to coordinate with us in advance so as not to create dangerous situations.
 
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MuricanSpirit

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I need fist to build a safe environment... eg. two carbon filter fans (one under the table) and some storage room under table. Fire extinguisher too. I already got some tubes as the one you showed in the pic - 2 with a straight glass pipe and 2 with a spiral pipe in the inside. I got a pump to cool the pipe down.

Of course gloves at the inside and outside.

What else do I have to check for a safe home lab environment? Slash protection; Tech outside; Fire extinguisher; Gloves; Chem safe lab gear (glasses, gas mask, chem safe jacket and pants, shoes/plastic boots, water protective ski mask etc.); what else?

I watched some youtube videos "Chemistry is dangerous" eg. I just learned 10min ago how to correctly/safely remove gloves. You are talking to an absolute idiot here.
 

William Dampier

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Do you have reflux condenser? Can you show the photo? Are there any flasks then?
 
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MuricanSpirit

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

But I have 2 like this:
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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.
 
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