Isomerization of CBD Isolate Using ZnCl2

Where are You located ?

Pennsylvania

1 Like

Regarding the first method of isomerization on the website:

Dissolve 1g of CBD in 10ml 0.005molar H2SO4 in glacial acetic acid.
Let solution stand at room temperature.
After 3 hours CBD has been converted into 52% delta-9-THC and 2% delta-8-THC.
After 3 days a mixture of 15% delta-9-THC, 54% delta-8-THC, 10% delta-8-iso-THC and 10% CBD has formed.
Work up:
Pour into water (100ml or more) and add cautiously with stirring (foaming!) enough sodium bicarbonate (15g should do) to raise the pH above 7. Extract with petrol ether, wash with water, evaporate solvent to get mixture of starting CBD and predominantly delta-9- or delta-8-THC with some other byproducts depending on the reaction time.

Do you think I can replace the petroleum ether with heptane? This is apparently 100% heptane: https://www.amazon.com/Bestine-Solvent-Thinner-Rubber-Cement/dp/B004O7HM38/ref=sr_1_1?keywords=heptane&qid=1555864175&s=gateway&sr=8-1

I am thinking this would be an easier method of isomerization.

Thanks.

1 Like

Switch it to hexane or ethyl acetate, unless you know the solubility of THC in heptane. Also, I would reflux this reaction so you aren’t waiting days for a garbage yield. If you have a pressure tube I would try that out too.

1 Like

Heptane should be fine. Most nonpolar hydrocarbons with suitable boiling points should work.
I’ve tried this isomerization with H2SO4 in acetic acid successfully, and used a low boiling white spirit for the extraction, since I had it on hand.

The isomerisations using Lewis acids like zinc chloride are also interesting, since they can produce higher THC yields than H2SO4.
I found a few procedures/patents online. The best one I found is patent DE10106024B4.

[quote] A solution of 5 g of cannabidiol in 1,600 ml of dichloroethane, with 10 g of zinc chloride is boiled for 24 hours under reflux. After the reaction is stopped with the addition of 500 ml of water. contains the product formed after distilling off the solvent residue

cannabidiol 2.87%
Iso-tetrahydrocannabinol 5.75%
Δ 8 -tetrahydrocannabinol 5.01%
dronabinol 86.37%
[/quote]
A yield of 86.37% delta 9 THC is by far the best I could find in any procedure.
It has a few drawbacks, however: One needs a ton of dichloroethane, which is a known mutagen and hard to obtain. Also, the reaction mixture needs to be refluxed for 24h.
I wonder if the dichloroethane is in fact needed, or if it can be substituted for another hydrocarbon.
Potentially, one could just use a non-toxic mix of hydrocarbons like white spirit with a boiling range of about 70-100°C, boil/distill off anything that boils below 84 °C (the boiling point of dichloroethane) and use the remaining solvent to carry out the reaction. But I have no idea if that will work, and one still needs to reflux a flammable liquid for 24h.

There are also procedures which use molecular sieves and heptane, also under reflux, e.g. in patent US8324408B2.
They form significantly more delta 8 THC, however.

For now, I’ll just stick with the acetic acid/H2SO4 isomerization.

7 Likes

Out of curiosity, does the THC mix/cannabinoid mix you isolate oxidize to form any colored compounds? The proposed oxygenated compounds that progress to CBN that have been isolated are all colorless compounds.

2 Likes

Interesting… Thanks for your reply

I have a question out of curiosity!

In this:

Post, it is stated that a molar solution of cbd and phosphoric acid can create a batch of d8/9. They talk about using clays but do not specify how much.

Would solvent be necessary in this reaction?

So those are 2 different approaches. The first is using activated acidic clays, neat. The hot distillate is stirred with clay in the still pot. The reaction proceeds to completion and the d8/d9 mix is distilled in good purity (we see 10/1).

The second method uses an acid or Lewis acid in solvent to effect the isomerization. There are multiple procedures. But solvent is used.

2 Likes

Hey, just by the way guys, if you can covert hemp to thc it’s 100% legal under federal law.

(b) Tetrahydrocannabinol.–Schedule I, as set forth in section

202(c) of the Controlled Substances Act (21 U.S.C. 812(c)), is amended

in subsection (c)(17) by inserting after ``Tetrahydrocannabinols’’ the

following: ``, except for tetrahydrocannabinols in hemp (as defined

under section 297A of the Agricultural Marketing Act of 1946)‘’.

If the cbd comes from hemp and the thc comes from that then the thc came from hemp. 100% legal and protected by the federal government.

1 Like

Is the federal government gunna represent you in court on that one?

5 Likes

You ever heat distillate or isolate to 150C?

It ain’t gonna be solid anymore.

1 Like

Read this patent closely. I read this a while back and was like, oh shit. They are talking about molecule purity of 97% for d9 with boron trifluoride
And sodium carbonate. If you read further down the conversion % was not all that impressive.

1 Like

very interesting… If CBD isolate is decarbed, but decarbed still powder, what makes it liquid after heat it for not coming back if it is not decarbxilation. I dont get this. So if I heat cbd it wont come back to powder after been coled? I would love to hear the explanation for this.

take sand, heat it up. it becomes liquid.

cool it down. what do you have?

it’s no longer a powder is it?

same concept.

edit: both can be ground down to powder, and the process repeated…

4 Likes

Instructions unclear, dabbed sand, seems safer than that time I dabbed some zncl2; but not enjoyable. 3/5 stars.

6 Likes

see…titanium nails do have their advantages.

3 Likes

Just tried for proof of concept, and this sand shit is bunk!

I was told it was made from the purest silica, and all I have is a tiny piece of beautiful glass… And a headache…

1/5 stars… Would NOT dab again

2 Likes

The reaction is a melt. Heat two solids up to the temperature of the sun until they melt together. It’s actually a VERY useful method of reaction. In this case, I wouldn’t have chosen ZnCl2, but it should work.

not so sure about the states but I know in the commonwealth

and I mean I know and have done this.

if you can show that the legislation is on your side no lawyer is needed.

in fact if you get a guilty as you were defending your self you

can instantly go for retrial as you did not have the education

of a lawyer and you showed the evidence in a way that was

not accepted in court.

this does not mean your evidence was false just that the ministry

of funny walks was not happy with your walk.

it is what it is and if the law states that you can cook like me

then the law states it.

you don’t need the bar to defend your self.

just the nerve.

i’ve beaten them multiple times fully red handed.

ive had qc and had to tell them to stop and do what the fuck

I tell them too.

you have to remember that no lawyer knows the chemistry

behind this stuff and therefor does not understand the law.

you must stand up for your selves.

and in fact for the rest of us as well as I have done multiple times.

the law is the law and ignorance is no excuse.

this is also applicable to judges.

hence the ability to step up to a higher court for retrial.

still I would not go via lewis acid my self.

remember there is a big difference between cooking your own

and cooking for supply.

they have made d8 illegal to sell in many us states from what

I have read here.

that is made from CBD so I would be real careful if I was selling it.

as a I make it for meeeeee.

well I think you could have a good chance with that.

also if you have a script your even closer to untouchable.

they fight to the letter make sure you know what that is and

if you can prove it then your fine.

remember the “intent of the law” it can get people

with out them even knowing.

but that is not the same as against the law.

1 Like