Thank you kindly @kcalabs I’ll dl the chain of custody and stick them in the mail asap.
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Left flask: Toluene ptsa 1% reflux at 80-90C 3 hrs.
Right flask: Hexane ptsa 1% (no reflux) rxn at 35-65C
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Best way to learn and perfect your skills is to dive right in! Looking good!
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You can make the toulene rxn look water clear like the hexane one in your photo or even nicer…just run @ rt for 24hrs…really you can get it fully converted in less time than that if your monitoring closely but that’s a safe bet. Also TAC when running toulene like this should be 95%+ assuming proper clean up and monitoring of rxn. -That goes for Heptane also.
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Have any coas to show this rxn? I’m wondering if there’s additional unknowns just letting it react that long? My rxn even when at rt always go to minimum of 65C I suppose one could ice bath if not using a jacketed reactor?
Also, according to our in-house hplc, I was only able to achieve 88% 8 11% 9 via toluene
Your in house analytics are from the hot toulene run @ 80-90C correct?
I’ve never seen temp climb that much from 1% of Ptsa in either Heptane or toulene begining at room temp…
Yes thats correct.
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This most recent run from today was using Hexane. First time I’ve tried a non reflux sop. As.advised by a few people on here, I tried the rt rxn. Still spiked. It wasn’t unmanageable, but it did what it did.
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The heat is bringing your TAC down I promise that much that’s about all I really know. Run room temp to compare. There are many methods using colder temps it would be interesting to run & compare to these other methods. That could look like 22-25C or ballpark room temp for 24+ hours medium-fast mixing…that could also be @ 0C for even longer @ 96+hrs medium-fast mixing should work well for both hept/toulene.
Then the anhydrous Ptsa seems to convert at much higher speeds than the ptsa mono so running that cold would be interesting. The colder temps should reduce byproducts & unknowns…however longer run times do also create these although again much more likely at higher temps. Since ptsa anhyrous is much more aggressive than ptsa mono and converts faster you may be able to push the rxn to completion at colder temps quicker with the anhyrous form. - I only played with anhydrous enough to know it converts way faster at cold temps and I didn’t have time to further explore that.
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Also Ptsa Anhydride is aggressive and converts faster than ptsa mono ime. So the Anhydride is likely worth exploring at room temp& colder temps as well for faster rxn times… anhidride is expensive though.
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Thanks for the tips and explanation. Yeah, I just make this for fun so I’m open to trying different rxn for the sake of just doing it. I’m going to start a heptane run tomorrow morning. I’ll put my.bf in ice once it goes for it to see if i can maintain control under 35C. I have a huge jacketed reactor, but don’t make this at scale. Small batch. I won’t be able to distil tomorrow though. Monday for sure
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By the way, im using mono.
Also will eventually make a huge run and put the crude into the wiper and see what happens. I just want to better understand what’s going on with it.before I waste another few kgs of this white dust.
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Keep it under 30C if possible don’t heat it at all run for 18-24hrs medium fast mixing somewhere in the 18-24hr period you’ll find the most optimal time to stop for complete rxn & high TAC. Too close to 18 hrs and youll likely have cbd left unconverted.
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Any plans on doing a DCM run?
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I’ve given it some thought. I’ve only handled it a couple of times. Have you used it?
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Worked with it but not for this application. I’ve never even attempted a d8 conversion at all. I only ask because @iontrap said it was their preferred solvent for THCP and because I’m curious about the solvent byproducts that could be formed using a halocarbon
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I’ve got thcp on my list, but im far from trying it. Time to use the ol searchy search.
May try pentane too.
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