It decomposes and indeed the exotherm is
There
But realize that there is only 20 grams pure tiba that needs quenching in that 4 liter volume
So slow water addition is very controlable
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2 wt% TIBA to CBD? 3 L of DCM or heptane, etc?
Have all your safety shit around properly. Fume hood, glovebox, etc.
Make sure youâve looked up how to put out a tiba fire. An extinguisher doesnât cut it.
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I am currently in the process of explaining to our ownership we need to up the safety game before I even consider buying these materials. Like most chemistry fields, all the cool shit that works really well is often dangerous to handle.
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Buy it in a 1mol solution .
Itâs more easy and safer to handle it.
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If they give you any pushback when it comes to your safety PLEASE stand your ground and dont let them pressure you into an unsafe process.
Your life is worth more than some converted d9.
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That is the plan. I am probably going to go with the heptane solution.
And to think my goal is not d9, but d10.
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D10 can t be achieved with tiba
Raney nickel maybe but I would start with base solutions
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What is the driving force of TIBAâs pyrophoric character? Is it ligand exchange with the isobutyl groups and a localized strong exotherm (in the presence of oxygen)?
The aluminum center is really very electron deficient and has very high affinity for oxygen. Think of Al2O3, a very stable oxide, essentially withstanding almost anything.
Probably the Al-O bond formation is so incredibly exothermic that anything close by catches on fire, including the reagent itself.
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That is along the lines that I was thinking. Best to know the animal before you try to hunt it!
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We get our argon from a welding supply company. Does anyone know if welding argon is very dry? Something to think about for preparation. I will probably give the company a call, but just curious if anyone has run across different grades of argon.
Probably not a very pure grade. Typically, bottled gases come in a range of purity grades, max levels of moisture and oxygen.
For organoaluminum materials these are the numbers I have seen recommended and I found these by following a Wikipedia entry and its references;
Moisture: < 3.5 mg/m^3
Oxygen: < 0.001 vol%
EDIT: This seems to come out to < 5 ppm moisture and < 10 ppm oxygen.
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Just throw a gas dryer on it. Theyâve got cartridges on Amazon
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Argon is not recommended. I believe it has too good of an affinity for water.
EDIT: Might have spoken too soon.
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Didnât Argon shown to be better than N2 for this reaction?
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Idk anyone using nitrogen with triisobutylaluminium
Most put a gas dryer on the inlet from the tank and run mol sieve in the reaction, from my understanding any water robs d9 yield
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Seems like both gases are typically supplied with levels below the limits suggested above.
Not sure about welding-grade Argon @Simo
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I think the bigger issue is to get rid of the moisture in the cbd isolate than that little moisture from argon .
Even bigger problem lies in the solvent used for the reaction.
Freshly distilled CBD can be considered anhydrous, I think.
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