Anhydrous ZnCl2 cbd isomerization

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Read all three sections on air sensitive techniques, most importantly the section on safety

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Yes, a Schlenk line is probably the best way to do air-sensitive reactions short of a whole glove-box reaction. Learning Schlenk line techniques without the equipment in front of you is going to be difficult. Buying all the correct pieces to assemble a Schlenk line will be difficult without prior experience with this type of system. There will probably be a couple hundred dollars just in clamps to hold up the Schlenk line manifold. I used this type of setup for nanoparticle synthesis in grad school and looking back on it, I would not recommend this setup to anyone without previous chemical experience. I almost caused an explosion by condensing organic matter into the cold trap that, unknown to me, also had liquid oxygen in it (this is only an issue when using liquid nitrogen). Another member of my lab group did cause a fire by exposing a pyrophoric chemical to air by simply turning a valve in the wrong order, pressurizing the flask he was injecting into, shooting his syringe full of chemical out into the center of the lab starting a fire. These types of problems may not be an issue with this ZnCl2 isomerization, but the problems you may actually encounter are hard to enumerate.

It is possible for things to happen in lab that could have never been thought of pre-lab. These problems can only be fixed with existing in-depth knowledge that comes from years or work in the field. Some chemists with years of experience still have accidents, horrible accidents that change lives.

Bottom-line, there is no shortcut for this type of knowledge. Reading forum posts and asking questions on here is not the correct path. Please be safe and do not take any unnecessary risks with your safety or the safety of those around you.

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Sorry, I replied to the wrong person! This was meant for @CrazyGoat

No worries, I couldnt agree more

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Just as something anecdotal. I tried this reaction in a couple different ways; thought I’d be inventive and stray from an SOP.

I’m not a chemist, and despite doing a pretty decent job of argon blanketing and keeping proper vacuum…

The reaction got fucked up. Mystery peaks ran rampant, there was all sorts of side reactions, and I figured I’d try a dab of the distillate …

My lungs completely closed up for 20-30 seconds, and for a good panicked half minute I was wondering if I was ever going to breathe again. I then had the worst cough of life for 5-6 hours and my tongue and teeth felt weird for a good week afterwards.

I turfed the run; but if theres someone inexperienced on here with less scruples would be unwilling to throw away a mistake. This shit can be dangerous, especially without tight parameters and proper equipment.

I’m going to go back to the SOP, and add in some chromatography afterwards.

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If running similar processes please pay/ask for professional consultation on safety/methodology from someone like @Photon_noir.
He was kind enough to provide me the proper rundown on reaction/cleanup/catalyst choice for one of my experiments recently. I am not a chemist. Only with similar guidance can I confidently create a new product that might be safe for consumption.

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D8 is easy :stuck_out_tongue:

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This route with zinc chloride/bromide is for making d9 but I’m sure we’d all love a safe and simple way for d8 if your willing to share.

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You are in the wrong forum for asking questions like this. No one is going to dumb it down for you for free here.

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He is clearly not American, you forget most of the world has very draconian cannabis laws and people have horrible access to low quality cannabis. Converting CBD is attractive if you look at it from that perspective.

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@IsolationChamberLab I see the whole picture now.

@CrazyGoat apologies for jumping on your case without fully understanding the situation.
BTW I am only 1st generation American… mis padres son de Europa.

I wasn’t paying attention and posted without reading everything first. Just seemed like a hazardous environment could develop using such ingredients.

@tweedledew ya D8 is easy

By other side, I won’t get horrified by the number of lenguages you speak, American.
(dont try now to lie and say you speak more than one)

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Please post pics of your set up when it’s assembled.

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Why would someone be using ZNCL2 ( which is used for d9 ) to make d8?

Everyone knows Tosic is the way to go for d8

They just don’t know what solvent to use or the reflux time

The sop I use to get almost full conversion is from @Photon_noir, and the clean up is simple.

Water washes will remove any tosic acid left after the reaction and if you run your reaction in a hydrocarbon then you can water wash immediately after

Here kids have fun

This is directly from that patent

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you could monitor by TLC pretty easily if you make up a CBD standard for yourself. I like the KOH test dont get me wrong, but once you get to lower amounts of CBD starting material (when the rxn is mostly done but not all the way) you might have a difficult time making a definitive observation with the beam test.

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You could degass the solution (if youre in solvent) by pulling vacuum until you see some bubbling solvent, then back fill with Argon three times. Thats about as much as I would perform for a hydrogenation so its about as good as you can do here. Once youre satisfied with your degassing, then begin heating the solution and let the reaction run. Argon isnt that much pricier than Nitrogen, sure you might want to go with dry argon for proof on concept work - if the reaction works try again with cheaper/wetter argon if you wanna see its toleration for water in that way, if that works then try with even cheaper yet nitrogen. But eliminating water at proof of concept removes a confounding factor, but it wont make much of a difference if you dont make attempts to dry your glassware/system before you even charge any reagents. If you suspect water is some sort of culprit, your attempts to eliminate its potentially confounding affects you must thoroughly ensure its not present if that makes sense. For truly dry work I’ve heated my glassware pretty hot and let it cool under a significant stream of dry inert gas (dry nitrogen would be smarter than dry argon since youre just pissing it away in this step without any reagents present).

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So the d9 reaction steps are similar to the d8 just switch the just change out the acid?

I mean even cbn is a reflux is a certain solvent / catalyst

D9 you need an oxygen free environment

D8 you don’t

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D8 is a simple chemistry procedure involving. 1 catalyst
Either tosic. Acid
Citric acid
activated carbon
Or one of the acitic bentonite clays
T5,T41,
It’s pretty straight forward with little preping
To make D9
There is a minimum of 2 compounds needed and a 3 is often used
Mol sieves to control the reaction and a high boiling point solvent
Miticulas prepping is advised
To do this reaction in as dry conditions as possible

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