Beads loaded beads molsieves or polystyrene

What is the ratio of beads to isolate? Looking to replace p-TSA and having trouble finding that bit of info.

I was using 10%, based on the amount of CBD.
This is a good starting ppint. I did not many runs, because it was not what I am looking for.
So not sure how it will scale up.
More beads equals increased surface area and should therefore only speed things up.
At RT my reaction was completed after a few hours.

Awesome! I really appreciate the info @Labwork ! My two main questions were catalyst loading % and run time and it seems you got em both! I assume you were running an alkane solvent? Also, did you notice much difference in performance as the pore size increased? My gut tells me it should increase speed of RXN, but I wonder if there is any downside that I am not considering. Did you have a personal preference?

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If you have experience with the pTSA reaction, than just replace pTSA with those beads and everything else can stay the same, to get a good starting point.
% of catalyst, reaction temp / time, ratios.
I did this rxn in toluene.

I didn’t notice any difference between those 3 beads. Differences may come up if you start finetuning your setup.
But I do have to say that I only used a flask with stirrbar and they turned into fine particels over time. Therefore the surface area increased and poresize was not that important

Usually you would use a catalyst basket for those beads to keep the spherical shape.

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Okay, I really appreciate the info! I can’t wait to get some in and start playing. I already shot an email over to Purolite, but is there a preferred distributor I could contact to get some ordered?

Edit: nvm if anyone is interested, just hit up Purolite. Sean was fantastic to speak with!

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I wonder if anyone has attempted a qualified guess so far about how unhealthy these ethoxy-HHC and iso-THC could potentially be.
Would adding zeolith beads to a ethanol/HCL conversion reduce the amount of those unwanted side products? @Dr_Jebril

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I’dont think so.
It may rather pomote the reverse. :grimacing:
Still, I don’t really know.

What is actually the reasoning behind introducing zeolith beads into a reacion mixture ? :thinking:

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There is a paper on the use of molecular sieves in cannabinoid isomerization rxn
Where the yields jump
My personal experience is IF youfind the right bead it will favor the rxn but pffff
Like many there are 1000 s of bead producers and each is different
All in all I can recomend buying quality beads from the petrol industry and not the alibaba versions
At least those did not disintegrate in most cases
3a is my favorite size and on some reactions it s a +
Be aware that using beads only makes sense with overhead stirring for the amounts needed are vast (600 gr) per kg cbd input

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Yes exactly, it is the paper on high D9 synthesis using ZnCl and the zeolith molsieves, that is why I asked if it might improve the reaction with HCl too.
I have tried the Zinc route once with ZnCl from the pharmacy and 4A beads from ebay with equal parts CBD and ZnCl and beads but it didn’t really work, probably because it was refluxing in a naphta with a boiling point around only 40°C (“Petrolether” from the pharmacy) so it still wasn’t finished after 3 days. The distillate was still yellow from CBD but had also quite a distinct Delta-9ish effect.
But it turned out, Zinc Chloride and Carbonate can’t be washed out and letting it sediment also doesn’t cut it so I would have to get a filtering equipment before another trial.

Do you know if filtering with celite and again on a 0.1 um teflon filter would get rid of the Zincchloride and molsieve dust sufficiently? Or could it maybe leave behind too much very small killer nano dust?
Do you know if this reaction actually produces the desired result, if run according to the patent, in boiling heptane? (It might be a funny patent).
Or with what reaction did you use 3A beads to your advantage?
You are right that the cheap beads from ebay turned into a mush under stirring together with the ZnCl and the flask was uncleanable in the end with what I had but could probably be reused as a reaction only flask. This doesn’t happen with more expensive ones? Was already wondering what justifies the very big price difference of the molsieves from proper chemical suppliers. Do you think the same named beads from different suppliers have different efficacy as a catalyst? Can you recomend a good source for them in Europe? (you are in Holland I assume).
Thanks for your help