converting THC to its acetate makes it psychedelic

THC gives an acetate (ATHC) which is as potent as THC. The mental effects are quite subtle and pleasant. Prepare ATHC by refluxing the crude distillate of cannabis oil with approximately 3 volumes of acetic anhydride. It is purified by distillation i.v. or with steam.
Cahn prepared ATHC thus: add 150 ml acetyl chloride (drop-wise with stirring and cooling) to 185 gr crude resin in 500 ml dry pyridine. Crystals may separate during the addition, or on standing a few hours at room temperature. Pour the mixture into dilute hydrochloric acid/ice. Separate the oil, then dissolve it in ether. Wash this solution with dilute acid, then with aqueous sodium carbonate, and again with water. Dry the solution with calcium chloride. Strip the solvent and distill the residue (240-270 C°/20 mm). The mixture of acetylated cannabinoids is separated by dissolving 2 gr in 100 ml benzene and chromatography over silica (150-200 mesh). Elute with 800 ml benzene. Combine the washings and the original effluent solutions, then strip the benzene i.v. to recover about 60% yield of light yellow oil. The material remaining on the column contains CBD and other cannabinoid acetates which can be recovered with ethanol and worked up.





more to come

The Cannabinoids

Cannabis' notorious resin is a complex mixture of cannabinoids, terpenes, and waxes, etc. There are about 100 known cannabinoids that occur only in hemp, with the exception of Cannabichromene, which is found in a few other plants. The entire hemp plant contains several hundred known chemicals.
The cannabinoids are thought to be formed by condensation of monoterpene derivatives such as geraniol phosphate with a depside-type olivetolic acid. This leads initially to the formation of Cannabigerol (CBG) and Cannabichromene (CBC) and their carboxylic acids, then to Cannabidiolic Acid (CBDA), which undergoes ring closure to form TetraHydroCannabinol (THC) and its acid (THCA). The latter decarboxylates to form THC. Other biogenetic pathways featuring CBC have been proposed by De Faubert Maunder and by Turner and Hadley.

The acids comprise up to 40% of the cannabinoid content of young plants. THC dehydrogenates to form Cannabidiol (CBD). THC is a primary psychoactive cannabinoid. The minor constituent Cannabiverol (CBV) possesses only about 20% of THC’s activity. CBD and CBN are not psychoactive, but they have valuable medical properties.

Many synthetic analogs of THC are more or less potent than the parent molecule. The dimethylheptyl derivative is over 50 times more active, with effects lasting several days. Some nitrogen and sulfur analogs also are psychoactive.

The total synthesis of THC has been accomplished in many ways, most of which are difficult. However, the extraction of cannabinoids, their purification, isomerization and acetylation are easy experiments for dilettante souffleurs who would possess this elixir.




Extraction

Cannabis must be dried be it is extracted, because it is not possible to remove more than 50% of the cannabinoids from fresh material THC-Acid is difficult to extract If you plant to convert the THCA to THC, the plant material should be thoroughly decarboxylated by heating it under nitrogen at 105° C for 1 hour before performing a solvent extraction.

Chloroform is the most efficient solvent for the extraction of THC from cannabis. A single extraction will remove 98-99% of the cannabinoids within 30 minutes. A second extraction removes only 88-99% of the cannabinoids within 30 minutes. A second extraction removes 100% of the THC. Light petroleum ether (60-80°) also works well, but a single extraction removes only 88-95% of the cannabinoids; a double extraction removes up to 99%. Ethanol also can be used, but it removes ballast pigments and sugars which complicate the purification of the resin Extract the dried cannabis with a suitable solvent for several hours at room temperature or by refluxing. Filter through charcoal to clarify the solution, then chill overnight to precipitate waxes, then filter the solution again. Concentrate it to one-half volume, and extract it with 2% aqueous sodium sulfate (to prevent oxidation). Separate the aqueous layer, and strip the solvent. The residue is crude hemp oil.

The odoriferous terpenes can be removed by steam or vacuum distillation. Cautious distillation in vacuo yields a fraction of crude red oil (bp 100-220° C/3 mm). This can be purified by redistillation or column chromatography. Use ethanol to remove the residue from the flask while it is still hot. Filter the solution through charcoal, and strip the solvent. Distill the residue to yield pure red oil (bp 175-195° C /2 mm). Distillation must be stopped if smoke appears, indicating decomposition. Because THC is heat-sensitive, it is preferable to isolate the cannabinoids by column chromatography. The simplest method of column chromatography is performed with ethanol and ether extracts of hemp on alumina, yielding two major fractions: (1) chlorophyll, CBD, and CBN, and (2) THC. A second, more difficult method is performed on Florisil (use 10 times the weight of the oil) with the solvent system hexane:2% methanol. This yields a doubly-concentrated, viscous oil which can be repeatedly chromatographed on alumina to separate the THC and CBD.
Isomerization


The potency of marijuana can be increased by about 50% simply by simmering a water slurry of the material for 2 hours. Add water as necessary to maintain the level. Cool and filter the mixture, and refrigerate the aqueous solution. Dry the leaf material at low heat. Drink the tea before smoking the marijuana. The effects are much more intense and last longer than those from the untreated leaves. The boiling water treatment isomerizes the inactive CBD, and decarboxylates THCA to THC.

Although Cannabidiol (CBD) has no psychoactivity, it does antagonize THC and produces other valuable sedative, antibiotic, and anti-epileptic effects. CBD can be isomerized to THC. If the plant is Phenotype III (containing mainly CBD in its resin), isomerization can double the yield of THC.

The CBD fraction of column chromatography can be distilled (bp 187-190° C/2 mm; pale yellow resin) to purify it. Isomerization can be accomplished with any of several solvents and acids. Alcohol and sulfuric acid isomerizes only 50-60% of CBD to THC; p-TolueneSulfonic Acid (p-TSA) in petroleum ether or other light, non-polar solvent will convert 90% of CBD to THC upon refluxing 1 hour at 130° F.

Reflux 3 gr CBD in 100 ml dry benzene for 2 hours with 200 mg p-TSA monohydrate until the alkaline Beam test (5% KOH in ethanol) is negative (no color). The Beam test gives a deep violet color with CBD. Separate the upper layer, wash it with 5% sodium bicarbonate, wash again with water, and strip the solvent. The remaining viscous oil should give a negative reaction to the Beam test. The crude THC can be purified by distillation (bp 169-172° C/0.03 mm), or by chromatography in 25 ml pentane on 300 gr alumina. Elute with pentane 95:5 ether to yield fraction of CBD and THC. Combine the THC fractions and distill (bp 175-178° C/1 mm).


Reflux 2 gr CBD in 35 ml cyclohexane, and slowly add a few drops of sulfuric acid. Continue to reflux until the Beam test is negative. Separate the sulfuric acid from the reaction mixture. Wash the solution twice with aqueous sodium bicarbonate, the twice again with water. Purify by chromatography, or distill (bp 165° C/0.01 mm). Any unreacted CBD can be recycled.

Another method is to reflux a mixture of 6 gr dry pyridine hydrochloride and 3 gr CBD at 125° C until the Beam test is negative. Wash the reaction mixture with water to remove the pyridine, then extract the mixture with ether. Wash the ether with water, evaporate the ether, and distill the residue i.v. to yield pure THC.

Similarly, reflux 3 gr CBD in 150 ml ethanol with 50 ml 85% phosphoric acid until the Beam test is negative. Work up the reaction mixture, and purify the THC.

Alternatively, reflux 3 gr CBD in 100 ml absolute ethanol containing 0.05% HCl for 19 hours. Extract the ether, wash the ether with water, dry, evaporate, and chromatograph on 400 gr alumina to yield:

(a) 0.5 gr 1-EthoxyHexaHydro-CBN (EHH-CBN: mp 86-87° C); elute with pentane 98:2 ether. Recrystalize from methanol and water.

(b) 2 gr THC; elute with pentane 95:5 ether. Repeated chromatography will separate the less polar forms.

(c) 0.5 gr EHH-CBN, eluted with pentane 93:7 ether. It can be isomerized to THC by refluxing in benzene for 2 hours. Cool the reaction mixture, wash it with water; separate, dry, and strip the solvent layer i.v. to yield THC.

CBD also can be isomerized by irradiation of a cyclohexane solution in a quartz vessel with a mercury lamp (235-265 nm) for 20 minutes. Workup of the reaction mixture yields 7-13% THC.

Budder= delicious space cookies

Is the 'Beam' test similar to measuring pH?

Sounds like soaking your Buds in Floor stripper to me... Like that GHB or whatever it is

That's all I need, something more complex than growing to do to my weed after harvest. Good post!

Too bad you're not buying Acetic Anhydride, Benzene, nor Petroleum Ether...

Only acetic anhydride is unavaliable for one and anyone can make acetic anhydride. To make acetic anhydride you need acetone and a ketene lamp to make ketene which when touchs water becomes acetic acid. once all the water is converted into acetic acid or if you start with glacial acetic acid as your reactant with the ketene, the ketene reacts with acetic acid and each becomes acetic anhydride. Honestly if he can purify the resins as well as he writes out how to do it he can pull it off. Personally I'd love to try thc acetate if only for that fact that it is a white powder that dissolves in water, what cop would ever think to test water for thc? then again I'm legal in my state.

On a personal note I have every confidence in being able to make acetic anhydride but I have no conficence in producing laboratory grade pure materials. There for I would never try this myself but I would love to see someone with more lab experience do it.

One last thing, why does it seem like people love to tell some one else they can't do somthing like the ghb statement ghb is not cleaner it is sold as such online as an attempt to hide what it is, its precursers are used as paint stripper but so are the same solvents big pharma had whatever prescription pills API that you have ever taken in. Don't think that just because your pill is white it was never dissolved in acetone or benzene or chloroform or some other "paint stripper"

PIP313 said:

Only acetic anhydride is unavaliable for one and anyone can make acetic anhydride.

Click to expand...

Couldn't you also use Acetyl Chloride? I think I have a source for that..

And instead of Benzene what about Xylene (Dimethylbenzenes)?

This is not something that would be worth conducting, seriously. Acetyl chloride, benzene, and acetic anhydride? Where do you plan to get pure granulated CaCl2 for the dehydration process, or pure HCl acid?

It's not a practical procedure for something that isn't on par with DMT or similar psychedelics. It's something I could do, but with the lack of information about it, why bother?
Also, acetic anhydride is NOT practical to synthesise in a home laboratory, let alone a university one. You're best off buying it.
Not trying to shoot anyone down here, but this is completely impractical.

Yep my brain hurts.....i'll stick with just rolling up buds and smoking them.....

That's some heavy chemistry there. Acid chlorides deserve some serious respect. I doubt the product would be worth the work up. Also you need to separate the product with chromatography. High temp vacuum distillations. This requires more equipment that a home chemist could realistically aquire. Let alone the reagents and the skills to do it.

Alright well I hope someone is still on this thread, like replying to stuff. Anyways, I have a question. What your talking about:Turning THC into ATHC through reflux and stuff. Is that the same as the old school method of making hash oil. I know a little bit of basic stuff about chemistry, furthur than highschool, but not quite organic chemistry. But anyways. This is the method I know of.

Dr.Atomo's Hash oil(Trying to use memory to give credit where credit is due, it was a pamphlet in the 60's-70's)

Anyways:
First, extract the THC from the plant. Method isn't important, as long as you use something that holds resins, and as long as the extraction is fluid.
Get Naptha, but the suspended extraction in a bong and the Naptha in with.
Put a hose on the bowl part of the bong going into a sink, or be outside while doing this, and blow the suspension out. All the good will be in the Naptha on top. Blow till as much of the resin layer is gone as possible, and mix in a drop (may have had measurements) of acetic acid.
Cook the actual weed it came from in a pan to ashes. Mix it in (to cancel out or absorb any extra acetic) Then filter it out.
(Now this is the ending the pamphlet gave)
Everything that was not in some form of THC will have changed into THC, then all THC will have been transformed into Delta 9 THC. So now you should have pure Delta 9 THC oil.


Is this the same as what your talking about? Again I've gone a little furthur than Highschool chemistry, just not any college and definately not at organic chemy level. I may just be being confused because the similar "Ace"

first off forget the resin in the bong

second acetic anhydride is not acetic acid and needs serious planning to make that ur not gonna do my point was its possible if you want to waste more time than its worth.

third take your plant matter wash with pure methanol (99%) quickly and distill the methanol with a distilling kit DO NOT BOIL AWAY IT CAN EXPLODE IF YOU USE A FLAME OR IF YOUR HOTPLATE IS TOO HOT.

then distill the resin into a clean flask, isomerise, wash, extract, distill, redistill

enjoy the purest highest thc oil your ever get

Resin in the bong?? That's just a separation method. Acetic acid is easy to make. You could make it on accident while making Cholorobutonal, if you mix wrong. And I'm not trying to make anhydride.

Will the method you just posted make Delta9 or just THC?

Some good, handy info man, but there is no way that boiling weed in water will cause isomerization, it WILL remove a lot of water sol crap, but thats all, to isomerize CBD needs the CBD in a solvent like alcohol, with sulphuric or hydrochloric acid at the correct amounts, the refluxed for some time for a 65 to 75% conversion rate, if using NON polar solvent you need triflouroactic acid or paratoluenesulfonic acid in the same method for up to 90% conversion CBD is the precursor molecule to THC and its not hard to rotate the CBD in to THC

Gotta disagree there man, methanol is a shitty solvent, why waste time and effort with this rubbish when MUCH better solvents are available. Hexane CANNOT be beaten for honey oil that wont BUST your lungs, chloroform is slightly better, both are GREAT. Methanol is nasty, partly POLAR shit, use a NON polar solvent for the best honey, and water wash, followed by an ISO wash and your finished, isomerization is only worthwhile if you have HIGH levels of CBD present, otherwise, its a waste of time!! 79.3% hexane gold!! Quality varies with how good your weed is!! I would put that up against any methanol extraction going, and it tastes great!! As for butane....nuff said! This methanol extract is 30 year old, outdated, dirty old rubbish, join the 21st century bud,lol

A methanol extract would have all the same problems as an IPA extract but worse since its more polar than IPA.
THC isomerization is really not worth the effort.

HA! I make my own acetic acid all the time.

Materials:

Large glass jar
aluminum foil
Cheese cloth
rubber band

wrap aluminum foil all around your large glass jar
pour wine into the jar to 2/3 full
secure cheese cloth over mouth of jar with rubber band


Wait 1 to 3 years (unless you have non-sulfite wine)

If you want, filter and store the results in an oak barrel for 6 months longer.