Microwave assisted ozone degradation of D9 THC?

I’m a micro scale hobbyist, and recently acquired a CEM Discover (microwave synthesis reactor). I was wondering your thoughts on small batch forced degradation to CBN using microwave processing and a glass 10um gas dispersion tube with 10g/hr ozone feed. This unit is able to maintain a temp set point via internal IR sensor, and I have adjustable wattage up to 300w with a reaction vessel of 10ml. Batch size would be about 5g as I just like to experiment for personal use.

I’m thinking I could just plop in some cryo qwet shatter, set it to 150c/150w, and let er’ oxidize. For personal safety, ozone would be directly vented outside from a vac barb on the glass reaction vessel. I also have an air exchange rate of about 25-30 cycles/hr, and air quality monitoring via a eagle gas detector just to be sure.

Now for microwave absorption efficiency I was hoping I could get away with straight concentrate added to the vessel but I have yet to do any testing as I’ve been quite busy. I did read somewhere ethanol can aid the absorption of microwave radiation and provide localized superheating, however without a pressurized vessel it may be of limited use for my intended purposes.

Finally to analyze the results DCVC would be utilized, and fractions analyzed with a UV-vis spec
that’s capable of 1 pt/0.3 nm scan speed and 2nm slit width for decent accuracy. I’m using DOI 10.1080/10826070500187558, pg.2378 as a ref for UV spectral data points on a 200nm-400nm scan.
I also have some comparative spectral data from 99.5% CBD isolate and the starting concentrate. I have a solid base on UV spectrometer operation and I’m getting better at deciphering fractions, however I still haven’t picked up a set of cannabinoid reference standards yet(kinda pricey lol).

Would love some input on my described process as i’m self taught and I’m just working with random ideas that pop into my head.

Thanks in Advance,

The Ethanol Man

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Super intruiged, certainly not knowledgeable to be of any assistance :stuck_out_tongue: I’ll cheer you on from the sidelines though.

You should be able to find the end results easy enough with a lab test though. Have you been able to successfully separate cannabinoids with DCVC before? How many passes do you usually need? 3?

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Super intriguied as well
I un the pure oxigen Uv light and patience setup :grin: With moderate results
So very interested to know your results
I am sure @Rowan can get lab reports on your test. Samples and if not maybe another member can help
Welcome by the way :fist_left:
Always nice to meet a like minded :+1:

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You should avoid ozone since it will perform an undesired reaction on CBD and THC. Not sure why people are using ozone for CBN oxidation.

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I don’t think you will see an isomerized product, but try it and see what you get. Either way it will be fascinating. @QGA where are you at’s?

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Dude I never realized ozone is o3 instead of o2

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People using ozone are just wasting their cannabinoids and destroying them.

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I literally just saw someone on here or IG talking about using o3 instead of o2 for more reaction lol

Thats funny

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They must be rich to be blowing through THC hoping to turn it into CBN with ozone.

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O3 destroys organic cells

Reason why I use it with a uvc setup to clean my grow rooms

Edit
Another reason why any live things can not be subjected to said o3 due to health risks

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At least it’s only a 5g sample size. I think the reason is there’s a patent that mentions it, but you’re right, it’s certainly not the logical end product.

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Thanks for posting, as I’m fairly new to chromatography in general my current separations are not the best. I only have a few runs down, but I was able to achieve a fairly nice separation in two passes.
I blended fractions based on the uv peaks, and definitely enjoyed the end result :grin:

I tend to learn best when i experience something first hand and experimenting with new things always adds a little excitement to the end of the work day. Currently I’m a little ahead of myself with some of my newer equipment but I always strive to learn all I can along the way.

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What’s your solvent gradient? I’ve had pretty good success with water/etoh in increasing parts ethanol

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I second WC’s opinion ozone is not going to a good option for being selective for thc, in fact I have ran ozonolysis reactions with cbd to cleave the tri-substituted olefin at the northern position following a selective adams catalyst reduction at the isopropene unit on the southern half of the A ring. The ozonolysis creates a new product set up for ring expansion aldol condensation to form cool 7 membered b-hydroxy ketones and enones. @anon93688

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Got structures on any of those end products?

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You would like the structures drawn or what?

More or less, can you please rephrase your question.

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Yes please.

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Thanks, I remember reading about your oxidization methods a bit ago and that inspired me to pursue this current path. I was hoping that ozone as a more aggressive oxidizing agent would provide rapid cbn conversion in a fairly pure THC sample. I would also expect the reaction time to be quite quick as direct microwave interaction has shown significant time savings in small scale studies. I def got some further research to do, and love the constructive criticism this community provides.

Nice to meet you as well :wave:

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Thanks for the advise, and I found this 60’s classic “Recent Developments in Cannabis Chemistry” - Alexander Shulgin. On page 5(401), he reported that ozonolysis of CBD lead to the generation of formaldehyde?

I’ve also seen HU-331 mentioned as a possible formation when oxygenating a cbd solution. I definitely have much to learn in regards to organic chemistry, and find it extremely exciting to find out the actual mechanisms of action.

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Thanks for your input as well, I’m very happy this community is so interconnected and happy to help.

Do you think oxygen would provide a decent end result using a highly refined THC extract, I was looking for a time efficient method for CBN, utilizing some of my newer equipment. I tend to mainly work with GRAS components for both my personal safety and peace of mind, as my analytics is strictly in-house atm. TLC, DCVC, and a Genesys 2 spectrophotometer is what I’m currently working with.

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