THC Acetate

[Gray Wolf]

Hi ya'll!

In response to a PM asking for basic procedure, we’ve only made three runs so far and are still shaking out the process but here is what we’ve done so far.

Disclaimer: Acetic anhydride and sulfuric acid are both highly toxic to breath and acetic anhydride is flammable, so good standard practice lab techniques for toxic flammable components are required. IE: Good ventilation free of ignition sources.

Acetic anhydride is basically vinegar with all the water removed, and reacts violently with water. Keep it away from water unless you are doing it on purpose.

Using an Erlenmeyer flask, weigh out and add the cannabis oil to the nearest 0.01 gram.

Measure out and add 2.5 grams of acetic anhydride per gram of cannabis oil.

Measure out and add sulfuric acid at 5% of the combined volume of acetic anhydride and oil.

Swirl the flask continuously for about five minutes and then cook in a water bath at 70/80C (158/176F), stirring the liquid occasionally for about 30 minutes.

After 30 minutes, cautiously add hot deionized water drop by drop at a ration of 2 ml per 5 ml of acetic anhydride. This reacts any un-reacted acetic anhydride.

Put solution in ice bath for about 15 minutes to cool.

Saturate dionized water with sodium chloride (table) salt until no more will dissolve. Add 10X combined volume of all ingredients.

You now have cannabis acetate.

Add hexane equal to 10X the volume of the combined liquids, excepting water. Shake well, and put in a separatory funnel. Allow to separate and bleed off the lower layers, leaving the enriched hexane layer.

Add additional dionized water and bleed off after separation to wash out the extract.

Cook off the hexane in a hot oil bath at ~250F and when it is bubble free, add ethanol to wash it out of the container and return to hot oil bath to cook off the alcohol and purge the residual hexane.

Smell the results and wash again with ethanol and cook off if necessary to get rid of the hexane smell and taste.

Bon appetite brothers and sisters, in that we continue to play with the procedure and have to date produced three different extractions, fortunately all impressive, yet all slightly different and we are still working out the fine details.

I will post the final results as those are available.

Hee, hee, hee, snicker, snark, snort…………

 

[spivak420]

?question?

?question?

Good point bro! The starting product was mixed trim and popcorn, which was respectable when vaporized.

The result was more than respectable and was an attention getter for the two of us high tolerance lab rats doing the testing yesterday.

We didn't test it Sunday, because the hexane was still purging. It was actually still not fully purged when we tested it, and today I will modify the process to include another wash using 190 proof to pick up the residual.

Gold represents it as 3X potency, which the two of us with our high tolerance were unable to establish, but I will put it out for panel testing to get more opinions.

Most noticeable to me was the strong head effect, because the pain just went away, which the straight oil also did admirably well without further processing.

More after I have run it by some low tolerance panel members to see those effects. My impression at this point is favorable enough that I will be making a larger batch for more extensive testing. Based on current data, I predict a highly postive response.

May I inquire as to where you procure Hexane?
I have searched high and low, online and in stores.
The best I have come up with is a website that sells it for $80gl.
To add to the obscene price they want a reason why a mere mortal would require such a product.
I get the feeling I will get sodomized by the Patriot Act if I fuck up my explanation.

Many thanks for your time and effort GreyWolf.

 

[GrinStick]

very stimulating, thnx

 

[Gray Wolf]

May I inquire as to where you procure Hexane?
I have searched high and low, online and in stores.
The best I have come up with is a website that sells it for $80gl.
To add to the obscene price they want a reason why a mere mortal would require such a product.
I get the feeling I will get sodomized by the Patriot Act if I fuck up my explanation.

Many thanks for your time and effort GreyWolf.

You're welcome! We get reagent hplc grade from our local scientific supply store, where we have a medical business account. Not cheap, but it doesn't take much.

Besides botanical extractions, Hexane is used to clean sensitive electronics. If you buy MB Electrical zero deposit contact cleaner, you will note that it is hexane propelled by a fluorocarbon.

Hexane is also used as a mass flow sensor cleaner in the automotive industry.

I'll bet a mere mortal wouldn't have much of a problem with a plausible use, as long as he looked legitimate and conducted themselves with aplomb.

By looking legitimate, I mean to not fit any of the profiles that they are on alert for. Mostly illegitimate drug manufacturers, terrorists, and those needing a keeper.

 

[Tr33]

good clean Hexane is also rubber cement solvent,
this leaves no residue when evap'd,
is cheap and easy to procure at your local art supply store,
not your dollar craft stores.
legitimate...artist don't need to look legitimate.

 

[juicepuddle]

removed

 

[spivak420]

You're welcome! We get reagent hplc grade from our local scientific supply store, where we have a medical business account. Not cheap, but it doesn't take much.

Besides botanical extractions, Hexane is used to clean sensitive electronics. If you buy MB Electrical zero deposit contact cleaner, you will note that it is hexane propelled by a fluorocarbon.

Hexane is also used as a mass flow sensor cleaner in the automotive industry.

I'll bet a mere mortal wouldn't have much of a problem with a plausible use, as long as he looked legitimate and conducted themselves with aplomb.

By looking legitimate, I mean to not fit any of the profiles that they are on alert for. Mostly illegitimate drug manufacturers, terrorists, and those needing a keeper.

Your prompt response is much obliged,
and your tip to not fit a profile, something more and more people these days are doing, is striven for on a daily basis.

 

[highonmt]

The acetylation of hydroxylated compounds is a classic medchem trick. As noted it is used to convert the dopamine antagonist morphine into the more potent and far faster acting ,thus more addictive, heroin... diacetylmormphine. The acceleration of onset is a result of the acetylated compound passing through the blood brain barrier much more efficiently than the more polar hydroxylated precursor. If you can find diethyl ether or methylene chloride (dichlormethane) these would be good solvent choices. Running this under inert conditions prevents atmospheric o2 from eating up you ac2o using excess ac2o will solve the problem. Also you could try this reaction neat using ac2o as the solvent and reactant and gently heating with a match while in a spoon... ha ha ha ...the classic kitchen recipe for diacetylation of morphine. Good luck and remember you are not running a selective reaction on pure thc. you're also acylating every other hydroxylated compound you have good and bad in your mixture and sending it into your brain, Good luck and be safe.
HM

If you need more specifics on the reaction pm me,

 

[eloquentsoution]

just sampled out two more patients, using the acetate from our second proceedure, one a high tolerance long time user. they both felt the higher strength immediately. we had just vaporized bud oil and wrex bud absolute oil. they felt acetate head over the first two samples/five oil hits. is it stronger????

hits me hard everytime i break into that vial..... and i have not been stoned in years, maybe ten.

Hey sorry to go back to the budder thing but I just wanted to make sure the right stuff was covered. It is my understanding that what makes budder so potent is that the process to make it ends up changing it into delta 9 from a delta 6 I believe, sorry if this is horrible and no help at all, I read this thread a long time ago and cannot recall all the details:

https://www.icmag.com/ic/showthread.php?t=21219

Once again sorry if this isn't helpful or is off topic, I just did not see it mentioned and thought it was worth a post.

i have read similar info as well as confirmation from our org chem skunk pharmer stating the higher rotations are more potent. have not hooked it to budder. how does that happen? documentation?

 

[Gray Wolf]

Hey sorry to go back to the budder thing but I just wanted to make sure the right stuff was covered. It is my understanding that what makes budder so potent is that the process to make it ends up changing it into delta 9 from a delta 6 I believe, sorry if this is horrible and no help at all, I read this thread a long time ago and cannot recall all the details:

https://www.icmag.com/ic/showthread.php?t=21219

Once again sorry if this isn't helpful or is off topic, I just did not see it mentioned and thought it was worth a post.

Not at all, it is a valid question, and my thoughts are that unless processing beyond the traditional buddering process is involved, I don't see how it would make such a delta conversion, but I am not a biochemist.

I will run the question by our dashing young biochemist brain trust for his thoughts tomorrow and pass them on.

From a practical standpoint however, I'm not sure that acetate will budder, given that it is runny, compared to ISO or BHO.

I have never had the pleasure of Budder King's budder, but I have yet to sample budder or oil that has the same uptake speed as acetate.

In actuality, at my tolerance level, I can't tell any difference between my own budder and the oil I made it from, other than handy packaging and the speed that I went through it.

Until I do try BK's product, my own budder experience and review on this forum leads me to adopt Occum's Razor with regard to Budder King Inc marketing literature, and believe that he most likely has cultivated an optimum strain for buddering, which has potent medicinal properties.

That is for sure what I would do if I were in his line of business and he seems to be staying in business, so I infer he pays attention to those sorts of detail, whether he is using the magic of modern chemistry to further enhance his product or not.

I'm inclined to try buddering some acetate just to resolve the question, but it is low on the list of other things we have scheduled to try with it, so I will have to get back to you on that.

 

[juicepuddle]

removed

 

[SacredTHCRitual]

this thread is awesome by the way.
probably as far as it can go on the ICmag forum without crossing the line into synthesis territory. THC chemistry is so fascinating and the knowledge is still so new. Today we look into these molecules the same way Galileo Galilei looked into the heavens. Make no mistake about it, the truth will only add good things to your trip.

The acetylation of THC would be great for people with chronic pain that need that instant kick on top of the long lasting creeper effects of a darker standard oil. If chronic pain is constant to where it is literally unbearable, the combination of diacetylmorphine and acetylation activated cannabinoids would be a prove to be an ultra potent mix. I was reading the other day how THC in high doses actually reduces morphine dependence.
( http://www.sciencedaily.com/releases/2009/07/090706090440.htm )

From personal experience, cannabis, specifically high grade cannabis oil or extracts, does reduce one's physical dependence on the opiates. I'm surprised doctors administer opiates without THC, someday it may become standard procedure to use them in combination.

Somebody brought up a great point above - the acetylation was not THC specific. This is something that would need to be studied. It is great that minds are at least getting turned onto the possibilities. Some may choose to use more strain specific resin contents high in THC over the CBD/CBN. great discussion that should keep going.

I don't see this becoming to popular in the cannabis clubs for a number or reasons. Even though technically smoking the plant material of cannabis is more health hazardous, the stigma of concentrates and chemically extracted combustible extracts will prevent this medicine from reaching the smoking majority at large. We can already see this in many counties in california cracking down on concentrates. The stigma is absolutely unfounded but when we start smoking acetylated bubbling wax out of a devils dick pipe its hard to say well hey its just weed man!. ha ha.
this swimmer smokes hash all day everyday if that says anything.
Groundless stigmas have probably done more ruin to society as history will show more than anything else but hey that's why we are here right now fighting for freedom of knowledge. cheers to that.

I was wondering if the acetic acid warped THC could be considered a rapid acting mild psychedelic? Not quite like DMT but definitely a rapid onset version of thc. It probably wears off quicker than the sedating standard amber oils. Wouldn't quite call it canna crack just yet but its treading that line. lol

I have seen good budder, all it seemed to be was whipped honey oil. With a slightly more butter like consistency compared to jelly hash. A pro honey oil maker showed me how to get budder right from the BHO tube. Easy: instead of evaporating in an open dish, this honey bee decided to evaporate onto a swallow tray of water. Water to oil derrr they separate. the honey oil sits on top of the water and can be purged by heating the dish with the water..then whipped in the tray and then scooped up with an old plastic card (the flimsy bevmo card is great). The budder is then allowed to dry (low humidity conditions preferred). Once dried it can be smoked as is, or mixed with a fine keef at 1/10 - 1/8 ratio depending on preference of consistency. some like to heat purge a bunch of extra times, re wash with grain alcohol, evap. whatever works for you. I prefer a hard oil rock or the budder. Above all would prefer a kiff that bubbled all the way. Where is Sam's 100% kiff method?

Something interesting to note, cannabis oils are flammable hahah. They really could fuel a car no joke. Even the most purged oils will catch fire if you don't vape them!!! hahah yes. someone else attest to this please.

So many different ways to use this medicine but I use a magnifying glass to vape my meds on a sunny day. Just a few drops on a little bowl clogger. good to go

 

[eloquentsoution]

yes, i will attest to the flammability of honey oil, but i am sure others have witnessed their oil flame when trying to roast a bowl laced with honey oil.

i have heard about running oil directly into water. if it is a small amount and will be used rapidly, no problem. but if you plan to store for any period of time you run the high risk of rancidity. any oil will go rancid with the introduction of moisture. it is why all skunk pharmers oil bathe their products and all cooks refrigerate oil water solutions.

in oregon, we are blessed by the legal luxuries of cannabis concentrates. the popularity of oil has definitely increased. honey oil is rx strength cannabis. there are varietal ways to make and use it, so many do and have experienced its healing properties.

acetylation, is another arena. it may have a medical use for fast onset, say for asthma attacks, panic attacks, ptsd and the like. beyond that, other esters will need much more r&d before even offering thoughts on potential.

 

[Gray Wolf]

Sooo, let's talk about the progress that we've made here!

Now that we have had an opportunity to make this enough times to get the same thing each time, I thought I would share the process with ya'll. Probably not refined as far as it can be, but works every time.

We started by dissolving 10.4 grams of BHO into 16.5 grams of hexane, to remove it from the storage container with an unknown tare, so as to not waste any left behind in films and to get an accurate weight. We warmed the mixture in a hot water bath to increase dissolution rate.

When dissolved, we decanted into a beaker with a known tare and weighed the total amount, from which we subtracted the beaker tare and the weight of the hexane to get the BHO weight of 10.4 grams.

We then poured that into a one liter boiling flask. To that we added 25 ml of acetic anhydride and 1.25 ml of 98% sulfuric acid.

We placed the boiling flask on a combination hot plate stirrer, and added a stirring bar to the mixture.

We added an Alhin condenser to the flask, through which we pumped ice water, and reflux boiled the mixture for one hour while stirring.

After refluxing for one hour, we added 40 ml of water to react the remaining acetic anhydride, and another 40 ml of hexane. We poured that into a separatory funnel, which we finished filling with saturated salt water.

After shaking well, we allowed the layers to separate and bled off the lower water emulsion layer, only to refill with salt water again and repeat the procedure until we had run about 4 liters of salt water through the mixture.

After bleeding off the salt water one last time, we bled the hexane mixture into a beaker and after filtering through a 0.2 micron syringe filter, we boiled off the hexane using the hot plate stirrer, with the beaker sitting in a larger beaker half full of water.

Just before the hexane was gone, I refilled the beaker to the half way mark with 190 proof ethanol and boiled that off. I repeated the alcohol wash three times to insure the removal of the rest of the hexane.

The resulting acetate is of a lighter color than the original oil and of lower viscosity.

Here are some pictures and my apologies for forgetting to photograph the separatory funnel in action. Next time...........

 

[kannubis]

True medical research & development at its finest, and great educational value to boot.
Thanks for the dedication and disemmination Gray Wolf, et al.

 

[dope_roor]

i want to sample!

very interesting read, always been on the mental back burner for me

 

[juicepuddle]

i want to sample!

very interesting read, always been on the mental back burner for me

 

[jump117]

Hey Grey Wolf, thanks for the interesting and informative reading, the joy that you once again gave us!

Did you neutralize the acid with alkali after refluxing?

I am very interested to learn about the impact of acidity on changes of the color of the extract.

 

[Gray Wolf]

Hey Grey Wolf, thanks for the interesting and informative reading, the joy that you once again gave us!

Did you neutralize the acid with alkali after refluxing?

I am very interested to learn about the impact of acidity on changes of the color of the extract.

No need to neutralize after all the washes.

I haven't sorted out the color changes with Ph yet either brother Jump, though my perception is that the higher the Ph, the less yellow and more red (amber) the color.

When we were neutralizing with NaOH, we got a darker (red) amber compared to the more yellow than we are getting now and Red hash oil is also made raising the Ph using NaOh.

Interestingly, as the Ph changes, so does water solubility and we did discover that super saturating the wash water with salt (sodium chloride, NaCl) causes some darker constituets to become neither salt water nor solvent soluble, and to stick to the insides of the separatory funnel.

They easily washed off with warm water later, so they were clearly water soluble constituets. and would have made the oil darker as well.

 

[ElRubio]

Interesting inputs both guys!

thx for all th info!