Have you confirmed your results via GC? Have you distilled it and then tested it? Making D9 is the easy part. Making sure it survives distillation is the hard part…
ok so i run the @EagleChem sop and i have to say that shit is kinda gnarly and unsafe. Im not even sure i beleive her based on the photos posted of her aqueuos washes and the temops she was suggesting
why the fuck would you suggest 5% alc3 in that little of of soplvent like DCM that cannot take exotherms like this reaction does
i have however run this in multiplle differnt solvent ratiois and amount of alc and the reactions always doeas the same thung and it seems the d8/d9 ratio is deceided in the first few mins and doesnt change much if at all during the reaction acording to my hplc
theres better and safer ways to run this and who cafres if it takes 3 hours instead of 30 mins anwya ?
Dissolve your alcl3 in dry dcm
Add this slowly I mean 5ml\min
You ll get into the 90s
3L dcm/1kg cbd 2L alcl3/dcm
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yeah d9 is showing 88 to 91% and that doesnt seem to ever change from what i can tell. I think 5% alc3 is way to much
Rogues right; a Dropwise addition of the DCM:alcl3 solution is warranted. Either use a metering pressure equalizing addition funnel, syringe pump, or peristaltic pump(choice of which depends on scale) to meter your flow rate and keep it consistent. Monitor your temps and modulate flow rate based on the exotherm, you want to ride the exotherm carefully as a warm fart will might as well make DCM reflux.
Alch3 is super hygroscopic and even when concentrated in DCM it will remain hygroscopic even though DCM is not miscible with water it’ll pull in all sorts of moisture. I feel like a lot about running this reaction successfully comes down to hardware and infrastructure, your systems need to be optimized for running inert and anhydrous, specialty systems for achieving such reaction conditions are warranted. Desiccants and dessication columns will also be your friend.
The reason this reaction loves to favor the d8 pathway is because when alcl3 is quenched by moisture; it undergoes hydrolysis and releases HCL and aluminum hydroxide; these compounds promote reaction conditions that will induce a double bond shift forcing the product to favor the d8 pathway.
It’s a fun method but there’s better more consistent teks out there. This method is not well suited for a scaled production environment because it’s too easy to mess up, especially when you have a few different operators running it.
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nah i dont need tfo do any of that and fiqured out away to run to completion in 3 hours with no exotherm
this is easier then then d8 as ive notice like i said your d9/d8 ration is decided in the first few mins
thetere no need for a addtion or metering funnel ewither -i dont think you should be running exothyermic reactions inb dcm its just asking for trouble
ive probobly done 25 to 30 bench top rxns on everyting from THCP to THCH and everythingh in between and and its all been consisten that the d9/d8 ratios aree all formed in the first few minuetes and can run saftley without an exotherm and be done in 3 hours
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Many ways to skin the cat we were hitting mid 90s with it, but every once and a while end up with a failed batch, the method isnt very robust.
We moved completely away from DCM as it’s fucking gross and might as well set your DNA on fire
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i mean we all gunna die
someday and i never volunteered to be on this shitbox of a plamnet anyway
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I’d rather not give my operators cancer, but likewise 
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im not forntunate to have operators - thats for rich people
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No it s not you will not consume all cbd with less when running cold +~ 0C
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The question is ,what we all want to know how you skin your cat.
Im Refering to the Coa you posted a while ago…
Greetings and respect to all.
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i mean no diesrespect but i have hplc data saying otherwiswe - this was done just because i hd some spare time and ran a bunch of smaller reactions i domt have a hores in this race other then curiosity
ran with argon and without argon and i have not seen any dsiffrence in yeild or ratios
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The solvent to CBD ratio is more important .
I can’t be the only one the giggled at this, the seriousness behind the humor is a perfect blend.
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the problem with drop wise is the alcl3 is not fully soluble in even dcm it will clump together in traditional addition funnels. Better to use granule by granule addition with an auger style addition funnel. I have mine hooked to a gear pulley controlled by temp parameters. You can also turn the aluminum chloride into aluminum acetate mid reaction to avoid the moisture problem and then wash that out. better yet, a peroxide and avoid moisture altogether. You can also use an amine like HMDS to protect the double bond shift. I doubt you and @Roguelab needed this help but I do admire you two are my favorite to read here. @oilburner1 its pretty mean to basically call someone a liar when all I did was try to give you a free way to make money? Here is another spoon for you since the first one was obviously not valuable enough. You need the inert gas to run to prevent the formulation of hydronium ions that are encapsulated during the quench if you dont you will get to the bp in distillation and have all of the trapped hcl run your hard work to D8. Your initial assessment of it not being needed is…incorrect to say the least.
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i never said it was not needed i said it could be donme with or without inert gas . Im talking a couole gram scale on these expierements and you should always run inert gas no matters what rxn you are doing. Its not mean im sorry its just an honest assement of the procedure and did you read the part that have no real interest in this other just to see and defiently not making money on anything you posted. I just think if you going to post and suggest that dillution rate you need to fully explain the danger of that exotherm. No matters which way you slice it is dangerous and members on this forum have blown up multiple reactors doing so. I know it doesnt seem like much but theres a responsiblty for peoples saftey because everyone might not have the knowledge that you do and why throws random spoons and withholding other parts is kinda meh. Do you want people hurting to make monry to use your spoons and incomplete sops and pump contaminated d9 because they saw what you posted on the forum and are desperate turn threr abundance of cbd into any kanda cash they can ?
\Just saying and no hard feelings
are you switching solvents after you quench ? because the pic you posted drfinetly looks like it
Just checked some old notes and you are right if rxn is preformed at RT with good temp control of exotherm
Completion can be achieved with 1% reagent alcl3 not recomended for the amateur thou
What solvent do you guys use now?
Chloroform at rt gives same yields
R134a also 