THC Synthesis From CBD Using Ultrasonic Bath

[Dr. MMX]

Beautiful idea

 

[Eleusius_hive_reboot]

I LOVE YOUR ETHICS !...feels good to make the experience of like-mindedness.... lets
show that we are not a bunch of degenerate thugs.... its the best counteract to the
authorities,being MORE professional and especially care more about the recipients health, of our

Products, than the corrupt big pharma industry..., (nice 4-methylmethcathinone-hydrochloride ....by the way, looks almost analytical grade)

 

[Dr. MMX]

Everybody has its job in the world

 

[rotovap5002]

This gives d8 not d9.

 

[William D.]

You are talking about synthesis without ultrasound. In which we get almost pure d8. Here we get a mixture.

 

[William D.]

Now remind the old Shulgin condensation (and others) from olivetol. What acid was used there to obtain d9? Yes, pTSA. You will obtain d8 almost pure without the use of ultrasound. Because with a more time, the d9 in the reaction undergoes isomerization to d8. This is the meaning of ultrasound synthesis. A shorter reaction time that allows you to keep this process to some extent.

 

[grävling]

Will make D8, with low D9 +-5%

 

[Rabidreject]

Hey am I meant to be vacuum distilling what I obtain before eating it?

 

[mycelium]

Yes, and not necessarily eating but you definitely want to distil it before dabbing it

 

[Rabidreject]

Okay. I ran one reaction at room temp with 3% p-tsa in DCM for 24h.
A second reaction was run with no solvent at elevated temps. I melted the CBD on a hot plate, chucked in the 3% p-tsa and let it stir for an hour. This was then dissolved in DCM.
They were both worked up in the same manner - water wash, bicarbonate washes, brine wash, dried over MgSO4 and solvent removed.

I have two oils. The higher temperature one is around 2.7g and is a sort of red colour, whilst the second one (unweighed as of yet but it looks like more oil for sure) is noticeably lighter in colour.

I will bioassay each of them once, see if there is any differences and then make more and this time do enough to bother with vacuum distilling it after.

 

[William D.]

5% pTSA
48hours for RT synth
You can add a little more acid, your stirring should be good if you do the RT synthesis.

 

[Rabidreject]

Oh that’s interesting. Ok so I didn’t use enough acid and I didn’t let it go long enough. Nice 1
Yeah I did have stirring on full as well

 

[Rabidreject]

oh also they were 5g scale reactions! Whoops

 

[Rabidreject]

Also I spilled a lot.

it worked though, is def active. Will make more so that vacuum distilling is more worthwhile.

 

[Rabidreject]

I will say. It’s a super annoying substance to do chemistry with.
Makes cleaning really annoying - or more so than anything iv done in the past and it’s just generally pretty annoying to handle.
I ended up doing a 20g reaction of this, I just need to distil it now but again, it’s an annoying task for me to do coz the noise.

 

[William D.]

The noise is really a terrible thing, I want to run away. Where there is something good, always burrow the pig

 

[ThaiLabWiazard]

Okay, so I think Its my time to share some info on this. As someone who has spent several hundreds of hours on this in the last year, whilst having access to analytics (HPLC). I have gotten quite a few interesting ideas of this forumn, and for this I believe its time to repriproicate.

So first of all the reaction pathway is as follows: CBD -> D9 -> D8.
Having pTSA as the catalyst (there are quite a few other options to choose from. A funny one I could share is conc. H2SO4. Full conversion in under 5 minutes.Beware exotherm tho) getting more than 60:40 d9:d8 is virtually impossible. Regardless of the temperature.

Unless you care about isomer-specific conversion of some THC homologues

Selective d9 is also possible but some more sophisticated catalysts. Like TiBAL (neither an advice or recommendation, just the original patent for dronabinol) or AlCl3 but under very controlled conditions.

Also the solvent seems to be not important at all to be honest. I recently discovered the possibility of Solventless conversion. The colour ends up red (as with H2SO4) but it is alright distillate.

As a bonus to everyone wishing to get rid of the red colour - dissolve the red product 1:2 w:v in ethanol and then evaporate under vacuum.
The red colour is caused by quinones <-> hydroxyquinones. The alcohol is a temporary fix, but for those skilled in art it wouldn't be a problem to think of a permament fix.

 

[mycelium]

Hey, thialab. I have never done the distillate thing but a lot of homeys have, and there is a whole website devoted to extracting cannabis, and nobody has come up with a way to stop the red ring, I believe it is oxidation, but I'm not a chemist...it starts at the top , and if one is using media bottles instead of quart jars, it happens less

I believe using toluene with pTSA ( instead of ethanol or methanol) can give a lot closer to 100% of d9.

But it is almost impossible to get one isomer or another.

A dude named " ion trap " who IS a chemist, said you can use chromatography, but that would be using so much muthafucking solvent and so much energy recovering the solvent that it would bee stupid

 

[ThaiLabWiazard]

Well, nope. Toluene + pTSA only gave me a 54% of conversion max. And that is after 48 hours of reflux... Tried it twice.

Ethanol and Methanol are a pretty nasty solvent, considering the acid catalyst.

It is 100% possible to get 100:1 d8 using any method, given enough time. D9 is much harder, but getting it pure is really hard. Since from the time of conversion, quench and purification. you are literally bleeding %. That is d9 converting to d8.

Preparatory chromatography is indeed a way to separate the isomers. But its economically inefficient. At least on the current market.

 

[ThaiLabWiazard]

As for the red "ring". Even after intert gas purging of the headspace of the bottle in which the distillate is going to be stored - it still occurs. IMO it is due to the viscosity of the distillate and the air bubble that get trapped in. They eventually rise to the top and the oxygen content is enough to cause the oxidation.