CBD Isolate to THC with muriatic acid (simple route)

[William D.]

Reagents: CBD isolate; Ethanol 96%; HCl35% aq.; NaCl; Water


Equipment: We used a reactor for convenience, but you can safely synthesize this in a beaker.


Yield: We got about 40g out off 50g, but you can collect more if you take your time separating the oil and use heat during the separation process.


Synthesis:
Add 50g of isolate to the jacketed reactor

Pour 1L of ethanol and stir until CBD dissolved. After dissolution, drop hydrochloric acid until to red litmus (pH ~ 2). Heat the mixture to 70*C and stir for 5 hours.

After 5 hours the mixture darkens a little. Pour the brine under the lid of the 2L reactor.

After 5 minutes of stirring, let the mixture stand and separate the resulting oil. It is better to repeat the rinsing procedure with brine once.

We send the resulting oil to an oil bath and slowly heat it up to 150*C. During the heating process, unnecessary components evaporate. In addition, the conversion of CBC into THC occurs.

After additional heating, we dissolve the evaporated oil in ethanol, repeat one wash with brine and obtain purified oil.

We recommend collecting the oil before the mixture has completely cooled down so that the product does not have time to thicken.

Since we did not use solvents for extraction, some of the yield is lost. But we did it this way to make sure that we could use a minimum of equipment for the best purity.

We will be happy to answer any questions you may have, enjoy!

 

[SoldadoDeDrogas]

I'm going to be attempting this experiment in a few days, when I get the CBD isolate, it's on the way. I will have to distill/dry my own ethanol to %96 from vodka.
I've been researching this experiment for some time and am having a hard time making up my mind with all the other methods including zeolite and the vast array of solvents.
Basically, I just want to get the most out of my CBD, so I believe I am aiming for the highest yield and ratio of d9 to d8 and spectrum. These instructions couldn't be much easier to follow.

So we can hope for around %80 percent yield of CBD into THC ? What is the isomer ratio of this particular method, how can we influence it? I am going for max psychoactive potency, of course :]
I know some of the hints for getting a better d9 yield include, trying not to let the temperature climb too high. Trying not to run the cook for too long. Trying to make the reaction as dry as possible...
is there anything else?

 

[William D.]

You can use dry conditions (using molecular sieves). To obtain yield, use additional solvents for extraction, and rinse the oil only in the form of solutions. For the exact amount of the desired acidity of the reaction you need to use a HQ electronic pH-meter. To determine the exact reaction time, analytical methods must be used. The above is the average. We do not have 100% pure in the end (there may be a regular set of impurities as iso-THC, ethoxy-HHC, CBC,CBN, etc). For purifying is better to use separation through vacuum short path distillation. The usual rotavap will not be the best solution, because you can have problems with distillation along a long path. Regarding the main cause of oil degradation, this is an increased temperature in the presence of acids or oxygen.

 

[mycelium]

I think that vacuum distillation of the converted CBD is necessary to make sure it's ONLY THC, as I read there are other side products formed(can't remember what....

 

[SoldadoDeDrogas]

I know it was recommended in the "CBD->THC 101" .PDF with the zeolite method. The "Coming soon 201" has to do with the distillation and stuff. I think that was more important for that method (or others with various ingredients) to remove all the solvent(s) and anything that got through filtering. With this one specifically, after the brine wash, the heating slowly up to 150c (for how long?) will evaporate any impurities, as well as convert CDC to THC. Followed by another brine wash.

What is left in the photo above looks pretty good to me. I wouldn't bother vacuum distilling that personally - it doesn't seem worth the effort or potential mechanical loss. But of course, that is the best idea for the best results. Getting only THC is important, but I want to make sure, also, that the THC has the highest concentration of the most potent isomer.

 

[mycelium]

Yeah I've actually seen someone's THC degrade on the second or third pass, trying to get it super clean. Based on the lab tests they did with every batch...
But I find it odd that it only converts to THC and not a little CBN or exo-thc, etc, like other THC conversions

 

[SoldadoDeDrogas]

Yea, the heat slowly degrades the THC from d9 to d8 to full spectrum, I believe. I don't wanna fill up the thread with a bunch of "I don't know" stuff, in case I'm wrong and my terminology is probably off, but I want to use the world selectivity, I think?. In other words, the CBD will follow a selective path when it does what it does. For example, I guess you convert the CBD before hand, and then run these reaction parameters (zeolite or lewis acid catalyst etc) on it to achieve the desired isomerization results for the different THCs and CBNs. Kinda like with your p2p for phenethylamines. For example, AlHg on p2p makes meth. P2np makes amph, mdp2p makes mdma and you can guess mdp2np.

 

[chost]

Hi @WillD
thanks for the tutorial, do you know what the ratio between d8 and d9 is?
And do you know if I change ethanol with IPA or methanol how much influence that has on the ratio?

 

[William D.]

Should be mostly d9 unless you hold longer than necessary. Use TLC to control reaction. CBD conversion is very solvent dependent.

 

[Rabidreject]

I’m going to give this a try when I get a few hours (well a day really but u get the idea).
My CBD isolate came today and iv been meaning to try out a few diff acids.
I also love the look of a jacketed reactor. They just look so cool - particularly when cooled with bright green/yellow coolant lol

 

[Rabidreject]

Didn’t seem to work at all for me. Refluxed for longer than the 5h because it didnt darken much. In the end I gave up after like 7h and tried adding the brine and I just got a clear layer of oil sitting on the top…

 

[William D.]

What color of oil is obtained? The time is indicated approximately, it may depend on the heating and quality of stirring. We will not say exactly for each case without analytical methods.

 

[William D.]

Unfortunately, colored coolant is not always convenient if you need to see the contents.
What acids do you have for conversion? Maybe I can recommend something with use outside of this topic.

 

[Rabidreject]

Alright so the oil obtained was a nice golden colour - there was just very little of it. Did a 10g reaction and received around 1g of oil. I cleaned it up earlier and ate a bit of it so I can see if it’s active. It’s certainly not poisonous as I’m working the dose up.

So acids I have - conc sulfuric, 32% HCl (is what I tried earlier), GAA, benzoic, phosphoric, fumaric, think that’s it.

My plan of action going forward was to use the sulfuric along with some toluene to whip up some p-TSA and then use that (either cooled or not) to make d8 or d9 depending on temp and length of reaction.

I was going to try citric but meh I think p-TSA is probably a better idea.

 

[SoldadoDeDrogas]

I did a quick test run on 5g of the CBD isolate. I am very impressed with the results. I got back 4ml+ of crude oil. Very psychoactive. I will be doing a 40g batch later on and will post that work up.
For the 5g test run I reduced the ingredients proportionally, so for 5g I used 100ml of %95 ethanol. It took about 20 drops of %37 HCl solution to get to ~2 pH on the color chart. I heated it in a beaker in an oil bath at around ~70c the temperature was in the oil. I swirled the beaker back and forth for a moment every 20 minutes to mix. I put a piece of plastic over the top of the beaker with a dimple in the center to reduce evaporation and loss of ethanol and collect drips of condensation during the reaction. For the 5g batch, after about 3.5-4 hours the color was a dark deep yellow/golden pee color. At the start of the reaction it is a very pale light yellow. This was a good time to pull the small batch. It took about two parts saturated brine to 1 part reaction mixture. It took a moment to settle and push the thc oil out.

I plan to run the rest of the 50g CBD isolate later and expect I will cook for the full 5 hours (or until satisfied with color.) I will post the results here. This is what the 5g cook looks like for now:

 

[William D.]

Try to avoid contact of the product with air. And measure pH so that it is not acidic. Then the product will remain fine.

 

[mycelium]

Fuck yeah bro. Hats off

 

[SoldadoDeDrogas]

Here is a quick update on the status on the bigger cook, I still need to wash the resulting oil. Anyway:
38g of CBD isolate was dissolved into 700ml of %95 ethanol, Everclear brand grain alcohol.
%37 HCl solution was added until ~2 pH was reached on the color chart while the solution was slowly heated to ~70c in an oil bath.
Temperature of oil and reaction liquid were monitored with a thermometer. A piece of plastic was placed over the top of the jar to reduce ethanol evaporation.
The mixture was swirled back and forth periodically for a moment throughout the entire reaction of about 5 hours.
The mixture darkens quite a bit after a few hours, and even more so still to about 5 hours at 70c.
After 5 hours, the color of the reaction liquid has darkened significantly, the reaction was left to cool to room temperature and brine was added about 2 parts brine to 1 part reaction mixture and mixed.
After a moment of mixing the brine into the reaction liquid, the oil pushed out and accumulated at the top of the reaction liquid. It was collected with a syringe for further processing.
~55ml crude THC oil was collected. I will continue to update this experiment. I must still wash the collected crude THC oil, heat to 150c and deacidify/wash again.

 

[William D.]

Additional advice. Before heating, you must measure pH. If it is acidic, you will harm.

 

[SoldadoDeDrogas]

I didn't see this until just now. Had already brought it to 150c for a moment in the oven. Last I checked pH was before I pulled it off the heat at the end of 5 hours, so unfortunately, I will have to do better next time. This stuff is extremely tough to work with, it cooled into a puck in the bottom of my beaker. It got a bit lighter in color and more translucent, extremely stringy trying to seperate a dab to smoke, it takes away the craving but I'm not terribly satisfied. I've been trying to eat a good bit to catch a buzz but I don't notice much there either.

 

[William D.]

Perhaps the conversion went further into less active substances. If some of the acid was in the remainder of the mixture. I think it is necessary to correct this moment for this synthesis or not to use additional heating without vacuum at low temperature. Your first successful experience without additional heating speaks of the same thing.

 

[CCL4 huffer]

ptsa or ACl3 give way way better yields due to the d9thc being hydrolised by the water in this reaktion and eaven those are quite tricky to get right im guessing u only endet up with a few mgs of d8 thc

 

[William D.]

pTSA is possible the best choice now.