Isomeration and extraction of THC

[borodin]

Hi!
I have found this recipe but i'm wondering if is possible in the Step #14 use another solvent less toxic than toluene. Isn't there a risk of contamination of the oil with toluene? Thank You!



"Fast and Easy Hashoil Production
Need to Print the Fast and Easy Instructions?
by The Watcher
Hello friends. I am going to try and relate to you, the real method of producing hash oil from the leaves of the cannabis plant.
Note: that if you are using flower of the female plant you will find an end product with at least 5 times the strength of the oil produced using the leaf of the plant. The reason for this is:
The leaf contains a low percent of the active compound tetrahydrocannabinol (THC).Which upon extraction from the plant will be mixed with a larger percent of the compound cannabidol (which the cannabis plant converts into the more active isomer tetrahydracannabinol by means of natural acids within the plant itself). So, by the process of isomerazation (which I will give instructions for in a bit), we will help nature along by converting the cannabidol into THC.
Now when you do an extract from the flower of the female plant you get a larger percent of THC than you do cannabidol. Now the THC being good to begin with you also get a bonus. The THC that is present will be converted to delta-9-THC during izmerazation which has a more pronounced psychedelic effect than the regular isomer of THC. (you also get some ungodly head rushes.)
So in conclusion, upon extraction and izmerazation from the leaves / shake / sun-leaves of the cannabis plant you have a large percent of THC which you converted from the cannabidol and a small percent of the delta-9-THC isomer which was converted from the already existent THC that naturally occur in the leaves of the cannabis plant. Now since there is a high concentration of THC in the flowers of the female plant and a noticeably smaller amount of cannabidol, upon extraction and izmerazation of the flowers you get a low percentage of THC and a much higher percent of the delta-9-THC conversion. This leaves you with a more psychedelic product when all is said and done. A bit of technical information taken from the solvent FAQ on:
TETRAHYDROCANNABINOL (THC)
found in marijuana, the psychoactive stuff
prop: bp 200 C @ 0.02mm Hg (other cannabinoids may have bp's lower than 185 C)
sol: polar solvents, acetone, alcohol’s, etc.
note: this is an oily substance, not water soluble
Well it is time to get on with the extraction of tetrahydrocannabinol and the conversion processes.....
A LIST OF LABWARE:
1 CONDENSER 300 MM JACKET
1 FLASK, FLORENCE (FLAT BOTTOM), 500 Ml
1 SEPARATORY FUNNEL 500 Ml
1 FUNNEL
FILTER PAPER
A LIST OF CHEMICALS THAT YOU WILL NEED:
ETHYL ALCOHOL / METHANOL (wood alcohol)
SULFURIC ACID (Concentrate 96 to 98 %(you can use a weaker acid but the delta-9 conversion is greater with the stronger sulphuric acid)).
TOLUENE
WATER
SODIUM BICARBONATE (baking soda)
NOTE: The most easy to find solvent for the extraction of the THC from the plant matter, is denatured alcohol which is ethyl alcohol that has been made Poisson with methanol (sunny side is a good brand of denatured alcohol). Methanol can cause blindness and death ! So don’t drink this stuff, and make sure when you separate the layers as described later on in this process, you don’t get any of the alcohol solvent layer in with the toluene layer.
Well, now that we have gathered all these solvents and glass ware, we will have some of the best hash oil in about 8 hours that you will ever find. So on to the process of extracting and izmerizing the cannabis essence.

STEP #1
You must dry your plant matter to a state where it will crumble into a fine powder.
TIP use your microwave oven, heat the plant matter for 1 to 2 min at a time then let cool, do this till it is completely dry. To crumble the plant matter, place it in a 1 gallon plastic zip-lock bag and proceed to crush it with your hands. This works very well.
STEP #2
Place the powdered plant matter into your 500 Ml flat-bottomed flask.

STEP #3
Add enough denatured alcohol solvent to completely cover the plant matter, so that it floats freely in the solvent.
STEP #4
Connect your condenser to the flask. (Connecting the condenser to a water source).
STEP #5
Now, slowly heat the solvent / plant matter to reflux. Let this reflux for about two hours.
STEP #6
Turn the heat off your reflux equipment, let every thing cool down to room temperature.
STEP #7
Remove the condenser from the flask.
STEP #8
Now add your sulfuric acid to the solvent / plant matter solution, use one drop sulfuric acid per 50 ML solvent used.
STEP #9
Replace your condenser to your flask and heat to reflux once more, leave it at reflux for 4 more hours.
Note: this is where all the magic takes place.
STEP #10
turn off heat, let every thing cool to room temperature.
Note: The alcohol will have a dark black color at this point, it will seem to be almost thick.
STEP #11
Neutralize the alcohol with sodium bicarbonate.(baking soda)
Tip: When it stops fizzing you will have a neutral or slightly basic solution.
STEP #12
Filter the solvent from the plant matter with the use of your funnel and filter paper.
Note: If you are going to be doing a lot of oil production you should get a filter flask, aspirator and a buchner funnel. See the watchers chemistry works for information on filtering.
STEP #13
Add as much water as you have alcohol/THC extract.
Note: Toluene mixes with alcohol in all parts so you will not be able to separate the alcohol/toluene layers if you don’t add this water.
STEP #14
Add about 1/3 as much toluene as you have alcohol/water to your flask.
STEP #15
Mix all this well for about 30 seconds.
Note 1: As the THC dose not want to stay in the alcohol/water layer it will move with ease into the toluene layer.
STEP #16
Now use your separatory funnel to sperate the two layers. (see the watchers chemistry works for information on this procedure.)
Note: The toluene/THC layer will be on top. Also the bottom layer should be a light green color.
Important: If the bottom layer still has a black color you should do steps #14 to # 16 one more time, but once is usually enough.
STEP #17
Evaporate the toluene/THC layer till you can no longer smell any trace of toluene.
Note: when the toluene has evaporated you will have left in the bottom of your glass baking dish a black oil with a slight spice smell.
Well people, there you have it the over night process for the extraction/manufacture of some of the finest hash oil anywhere."

 

[thujone]

i think toluene is actually the safest solvent to use in this case, but don't quote me on that.

people who are generally paranoid about combusted solvents causing them harm will mix the final product with alcohol to dissolve it again, then equal amount of water and place it on the stove top to boil it all off again on the lowest setting.

but since i don't want to be held liable should you singe your eyebrows or blow up your house, i'll move this topic to advanced drug discussion where the real chemist eggheads can shed light on the true nature of this experiment.

 

[MurphyClox]

Now toluene isn't indeed THIS toxic and if one uses indeed sophisticated glassware, including a refluxer, the whole experiment is relatively safe.

Although there are less toxic solvents out there for the extraction/isomerisation, one needs the high temperatures for quantitative conversion of CBD to THC (check the boiling points of tol vs. hexane vs. DCM).

Murph

 

[Jabberwocky]

so can I boil this stuff outside with an electric heat source and a couple of beakers?

what about the filtering step, can I do that with a coffee filter?

 

[MurphyClox]

Nope, simple beakers won't make it, because you're going to lose too much solvent. A setup including a reflux condenser is HIGHLY recommended!

Coffee filters for the filtering step are OK but not the best. In my experience, they get clogged quite fast.

Peace! Murphy

 

[fastandbulbous]

You can use isopropanol under reflux, but it takes a hell of a lot longer for the reaction to complete (dissolved in isopropanol & 3 drops of conc sulphuric acid for every gram of hash oil. Reflux for 6-8 hours and Robert is your mother's brother.)

Rather than using filters, I always found adding lots of water (with a little bicarb to neutralize the acid) to precipitate it out, after both water & alcoholic solution had been chilled to 0'C caused the cannabinoids to precipitate out in a highly resinous form, so you could actually just decant off the liquid after leaving to settle (still at 0'C) for a while

 

[headymeds]

get a PVC pipe with one whole at one end small enough to fit the tip of a butane can in there NEON BUTANE IS MOST EFFICIENT
REMEMBER THIS IS A DANGEROUS PROCESS NO SMOKING NO FLAME DANGER!!!
and 5 holes on the other end of the pipe
grind your product up to a powder almost
i use a blender since i try and put decent amounts in it
well use leaves stems buds whatever has thc,...
DANGER DANGER FLAMMABLE
blast the butane through the one whole onto a Pyrex dish
it should all just ooze out into a yellowy honey color
or some may be black i have come to find out*still potent) but i havent seen the black in a while
well when its all on the dish you should already have the stove going at boiling temp and p ut the dish on top for the butane to evaporate
and just scrape it off with razor blade and find something to put it in
you can also put the dish in the freezer if you wana save some
and just do the boiling water again
this is danger i would say before using my advice read it a couple times and go on erowid or something to find a more thorough run down of what to do
i love this shit though SO SO GOOD i only smoke it on weekends or special occasions

 

[the better green]

^ that is the easiest method. I have used that method many a time. Infact, the PVC tube i use is nick-named the Hash Bomb 3000.

Anyway, theres one exception. DO NOT PUT THE BUTANE CONTAINING MIXTURE ON ANY HEAT SOURCE!(ie, NO STOVE!). Butane burns off at room temperature. If its 70+ outside, it'll evap right there, if its cold out, bring the dish inside. It will evaporate with no heat source. Putting butane on the stove is asking for trouble.

EDIT*

Ok i will clear this up a little better for you.

Get a pvc tube, with a 2 inch diameter, about 1 1/2 to 2 ft long.

Get 2 tight fitting PVC caps for each end.

Drill one hole in one cap in the center to fit the nozzle of a butane container.

Drill a few holes in the other cap towards the center of the cap.

Fill tube with grinded plant material (stems, leaves, seeds, buds, whatever)

Take some cheese cloth, or similar thin material, and stretch it over the pvc tube where the cap with multiple holes is going to fasten on. (this is to keep plant material from getting in the oil)

Hold pvc tube straight up, over a glass dish. Multiple holed cap facing down.

Empty a few ounces of butane (depending on how much plant material there is) into the tube through the single hole in the top cap.

After a minute or two, the butane will re-liquify and literally 'rape' the plant material of THC. It will then leak into the glass dish.

Again, it will evaporate at a very low temperature (i believe boiling point for butane is something like 50 degress or something low like that) so no need to add any heat source what so ever.

Scrape the oil from the plate, and voilia, easy hash.

Like the previous poster said, BE CAREFULL. NO SMOKING. BUTANE IS FLAMMABLE!

 

[phase_dancer]

Like the previous poster said, BE CAREFULL. NO SMOKING. BUTANE IS FLAMMABLE!

Also, never underestimate the potential for static buildup/ discharge. Performing the extraction on a humid day is advisable.

 

[MurphyClox]

The idea to increase potency of cannabis-derived oils by refluxing in presence of catalytic amounts of strong acids (normally toluene + H2SO4) is well known. The theory goes that cannabidiol is converted into delta8/9-THC. Well, all clear so far.

But I just found that delta9-THC itself decomposes upon longer contact with acids. As usual, elevated temperatures increase decomposition rate.
Ref: J Pharm Sci 1974, 63(10), p.1563

Let me just quote one sentence from the abstract:

The half-life of delta9-tetrahydrocannabinol is about 15 min at 37°C and pH 1, typical stomach conditions.

I think, that sheds some new light onto the "isomerization=potentiation" issue. Don't ya think? How much THC might be lost for the sake of converted cannabidiol?

Murphy