A nudge in the right direction would be greatly appreciated. So to start it off I am by no means a chemist but I learn pretty quickly. I’ve built our Hydrocarbon extraction lab from the ground up and pieced together some pretty efficient distillation apparatuses, Im very well versed on the extraction side from Biomass to Isolate. with the crash of the CBD market I have been looking at other avenues for our extracts and the one that peaks my interest the most is CBD-D8. I’ve ran a few experiments and built a reflux unit but I can’t seem to get it free of Delta 9.
here’s what I’ve done so far:
1: 14% by mass anhydrous citric acid to isolate in a short path, heated to 175c for 4 hours,
pulled vacuum down to 1000 microns to remove citric acid, distilled as normal.
yielded 50.56% D8, 22.94% D9 1.49% CBD remaining with approximately 25% unknown but according to Gobi labs there is a peak right before D8/D9 that they think is a neutral cannabanoid.
2: 10% by mass anhydrous Citric Acid to distillate, re-fluxed for 6 hours, moved distillate and Citric acid mix to short path, added 4% AC (Aquarium Masters Lab Grade Activated Carbon) short path as normal. yielded 37.97% D8, 26.87% D9, 4.18% THCv and 1.17% CBD remained.
I would really like to make this work with Citric Acid if possible so a nudge in the right direction from you guys that are smarter than I am would be greatly appreciated.
unfortunately i cannot provide you with firsthand information that someone here probably can, but I’d just ask have you tried holding everything constant and repeat experiment 1 at say 200C? or maybe 8 hours at 175c? i think it would be really telling
I will try 175c for 8 hours tomorrow. 200c is to hot I believe.
I can’t seem to find the thread I was reading earlier today about D8 conversion. They were talking about refluxing anywhere between 180-186 for 4-6 hours I believe. They were using CBleach though. Just a thought
Sorry wrong thread
I would think you’d see more conversion over time. let us know!
Next time reflux with ethyl acetate and a bit of hcl.
I accidentally converted cbd to thc doing something similar when I was experimenting with a different technique. I noticed very slow rxn rates until I hit 170C or so, for what it’s worth. Definitely hope someone can build off of that.
Can Ethyl acetate and HCL be removed via vacuum purging or would I need to do a wash?
Wash then distill. If you don’t neutralize after the conversion you get side conversions.
Thank you. Ill have to grab a separatory funnel or possibly try to use my chem glass 5L reactor. Its been just collecting dust for a while, would love to put it to work.
You think just dissolve the reacted isolate into Hexane at one to one then add water/salt mix at one to one and possibly some baking soda to adjust PH?
I preffure iso propyl but Yeah
@spdking I hadn’t considered ETOAc. It’s used to decaffeinate coffee. Ethyl acetate hydrolyses to give acetic acid and ethanol.
I did a few experiments with Methanol and Iso Propyl and they both dissolve citric acid, Hexane however wont dissolve citric acid.
I did a wash with Methanol/water and hexane yesterday which shows promise.
I believe the Cannabanoids would be more likely to go into the Hexane vs the Methanol/water with the citric acid favoring the Methanol/water mix.
Yes Unless pure methanol the cannabinoids have a slightly higher affinity for methanol
But as soon as some water is pressent it will loose affinity fast
This is for acitic cannabinoids by the way
Thank you for the clarification. I’ve been doing the majority of these reactions with Isolated CBD. Citric acid seems to work well at removing the Hydrogen from the oxygen atoms at the bottom of the CBD molecule but controlling the placement of the double bond at the top of the THC molecule is proving to be hard for me to control. Possibly to much energy input is bouncing that double bond back and forth I guess? I’m no chemist so I’m learning through trial and error.
Lol. Flashback of everything I used to make special potions… In the 80s everything under kitchen sink had one of those stickers.
Have you tried T-41 clay?
Yes. It didn’t really do a selective conversion.