THC Chemistry

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Prometheus

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This seems like the best place to post(since no one else is posting on this stuff),so hear goes.

Does anyone have any expirience with extracting THC, then activating the other Isomers to increase potency, ala cannabis alchemy. Hands on expirience is preffered, but any thoughts will suffice. I used to have the book years ago, but dont remember everything(and am not going to buy the book again). If anyone has the book and could post the synthesis and following procedures for activating the dimer isomers(I think there called dimer isomers anyway), I would be forever grateful. Also I will share all information about the synth if it goes all right(if anyone even cares)

I am hoping to make the process easy and more acsessible to the rest of the MP community, because I dont remember it being super hard, just intimidating from all the big words. I am hoping to finally be able to contribute something back to the group that helped me through my first grow.

Thanks guys, all thoughts/comments are welcome.
Happy holidays.

Prometheus
 
The book you need is:

Cannabis Alchemey; D. Gold ISBN#0-914171-40-2


It's been a long time, but if I remember correctly, it has several methods that are discussed in detail.
 
i wish i had these book before christmas....i woulda asked for it...thanks for the title Stoney :cool:
 
Thanks hick, like stoney said, you rock.

That article refreshed me very well. First things first, I need some pure hash oil. Stoney you have read my other post, I extract with pure Dichloromethane(DCM). It makes good strong oil,better than alcohol(any type, anhydrous or not),but not as good as butane. I think my DCM honey oil is probably good enough for the Isomerization. But, I dont have a problem spending the extra cash for some butane/dry ice and a homemade Dewar condenser. Do you or anyone else for that matter have an opinion on weather or not this extra labor is nescasary. I mean how important is the cleanliness of the starting precursors in this reaction.

Thanks for all the help guys,

Prometheus
 
Hey Prometheus, good luck on your experiments. I use Cole-Parmer for all of my lab equipment needs.

www.ColeParmer.com

They have good prices and good equipment selection.

You name it, they've got it.

The catalog is 2,408 pages with over 60,000 products.
 
Thanks for the link Stoney but, I have already obtained all of the nescescary equipment(I have had it for years in storage). I have mag stirrer/hotplate,flasks,distillation rig,etc. I do need to buy some keck clamps and a couple ring clamps, do they sell to individuals?, most big name science houses dont sell to street punks. Oh well there are other ways, however.

On another note: Upon re-reading Mr Hicks link, I noticed farther down the page. One poster cites the use of Acetone as his solvent of choice, Prometheus has no past expirience extracting with this solvent, does anybody out there use this solvent currently or in the past. Is it superior to alcohol?, if so how much more?(be descriptive, so I can better compare it to the DCM I am using).

As always thanks in advance guys, this may take alittle while but I am going to get this project done.

Prometheus
 
Prometheus said:
Thanks for the link Stoney but, I have already obtained all of the nescescary equipment(I have had it for years in storage). I have mag stirrer/hotplate,flasks,distillation rig,etc. I do need to buy some keck clamps and a couple ring clamps, do they sell to individuals?, most big name science houses dont sell to street punks. Oh well there are other ways, however.

On another note: Upon re-reading Mr Hicks link, I noticed farther down the page. One poster cites the use of Acetone as his solvent of choice, Prometheus has no past experience extracting with this solvent, does anybody out there use this solvent currently or in the past. Is it superior to alcohol?, if so how much more?(be descriptive, so I can better compare it to the DCM I am using).

As always thanks in advance guys, this may take a little while but I am going to get this project done.

Prometheus
Yeah, I've ordered as little as $7 of plastic from them. It's a new world out there now. Even the big ones will most sell to you now. It's all in the bottom line.

The Acetone is used because of it's easy and total extraction later. You don't want to be smoking solvents. Hhahahahaah, bad taste!

If it's done properly, the Acetone is completely removed. No trace.

Good luck man!

I researched making a still awhile back and found that it's a 1st degree felony in the USA to even have the equipment for distillation in your possession. What a laugh. USA law is fickle.
 
hey guys im just wondering have any of you all made just oil in the first step. as the whole idea of trying to acquire petroleum ether sounds quite sketchy to me not mention the explosive idea so anyway if so what are your experiances. good bad? and also has anyone tried this pure form of oil before. how does it work in relation to the prior. in the article he makes it seem as though there is no comparison. i find it very interesting and would love to try to make some because of my experimenting side. but would be too intimidated to try. but prometheus i would love to hear any of your results and thank you in advance for any future info
 
hey check this thread out from mjp there is alot of info and i mean alot about this exact subject i read all 9 pages and am kind of convinced that the acid idea will not make a huge difference from just plain oil. oh well its a good read with good posts from some very intelligent people http://www.mjp.com/ic/showthread.php?t=39661
 
learnin to gro said:
http://www.mjp.com/ic/showthread.php?t=39661
Very nice man! Here's a place to get a nice manual filter pump, the flask and beaker for reasonable prices. I couldn't find the #50 filters on this site tho'.

The acid and the bicarb I'm not sure where to get.

CLICK HERE
 
Sorry for taking so long to respond, I had to go back to work.

Petroleum Ether is not as hard to get as "they" would like you to think. Petrol Ether is a name given to an entire family of chemicals that are all very similar(if I remember right,the main diference is the boiling points, but the parent hydrocarbon is still the same) in chemical properties. Every time that I have encountered a synth that called for petroleum Ether I went to Lowes, or Home Depot, and got a can of VM@P Naptha. Naptha is one of the most common forms of Petroleum Ether available(brand name RONSONOL is also an exceptable substitute,Colemans or other store brands should not be used,since purity can not be guaranteed),and works great, for almost all basic organic lab work.

I have concentrated H2SO4 ordered and on the way, and it should arive sometime after the first of the year. So we are going to extract some crude starting material in a few days, and get this SOB rolling. I am curious to see how easy this process really is.

I promise Ill keep yous guys updated as I go, because this is already too much fun. I just gotta see if this **** is really, worth it?

Prometheus
 
Prometheus said:
I just gotta see if this is really, worth it?

Prometheus
Keep my uncle in mind. The man was a dedicated, informed scientist with a Doctorate in Physics.

In an experiment gone wrong, he ended up being something washed from the walls, ceiling and floor of the lab he was in.

Be very careful. This is only smoke we're talking about.

I hang it, I cure it, I smoke it.

My lungs aren't wild about the transaction, but other than that, I haven't risked much.

I don't want anyone here to think this is something to do with no knowledge of lab procedure.

On the kitchen counter while supper is cooking isn't something I would want to make this sound like.

Whisking with an egg beater in a Rubbermaid bowl is not the same thing as "agitate briskly in the beaker".

Yo! People! Be very very careful with this type of thing, OK?

Blind is blind. Dead is dead.

You get my drift. Use all that safety stuff. Face shield, apron, ventilation. Be smart.

If your high, stop messing with stuff until your not high.

Be cool folks.
 
Sorry for taking so long to respond guys, the holidays were a busy time for Prometheus, but the ball is rolling now so here is where we are at:

Recipie calls for 100% sulfuric acid, thats not really doable, its hard to get and is a constantly fuming acid nasty substance to work outside of a fume hood(wich I havent got). I got 98% concentrated H2SO4(the strongest commonly available acid. Even though that it is not anhydrous, me and others I have consulted think it will suffice.

My extraction solvent of choice DCM(DiChloroMethane), went up in price to ninghteen dollars a liter, so I am going to use either, dry Isopropyl or dry acetone(Im still in the air on this one).

I plan on doing a secondary super critical extracion of the oil from the first extraction with butane, so a make-shift Dewar was made(more on that later).

A Soxhlet extractor is no longer available to me so a basic reflux set-up will be used instead(this can also be easily and safely home-made, if anyones interested let me know Ill explain how).

The plant matter being extracted, is trimmings of leaf and loose bud from my last grow of sinsemilla, and is of good enough quality for these expieriments.

All the nescesary items have been bought and had, and I believe I am ready to start.

Outline of Procedure:
  • Construct Dewar condenser, from stainless steel thermos
  • Prepare anhydrous magnesium sulfate, from drugstore epsom salts
  • Prepare anhydrous extraction solvent (acetone or ISO)
  • Reflux plant matter with solvent for 24 hrs
  • Filter entire mix, strip solvent
  • Condense butane in homemade Dewar to collect
  • Extract crude hash oil with butane in dry ice/ ISO bath for 30 min, with aggitation
  • Strip butane, collect very pure hash oil
  • Disolve hash oil in 5-10x volumes of VM&P Naptha
  • Add concentrated 98% H2SO4, reflux
  • Neutralize acid, wash solvent/oil, strip solvent to obtain pure oil
  • Test oil
This is the procedure I have decided to use in my expieriments. I believe I have covered everything, but I will review the literature one more time before proceeding. I am going out to the bar tonight, so I will not start tonight. I will begin in the morning and work through the weekend to try to finish before i have to work on monday. I will post updates and clarification of certain procedures as I perform them. So stay tuned. Wish me luck guys!

Your pal,
Prometheus
 
Alrighty then, its almost dawn on saturday morning, and I am finally starting this damn thing.

First Ill go over the prepatory work I had to do to start:

Anhydrous magnesium sulfate was prepared using the following method: Drug store epsom salts were purchased, my oven pre-heated to 300 degrees farenheight(spelling?). I covered a CLEAN/DRY cookie sheet with about 1, to 1 and a half centimeters of epsom salts(exact amounts are not critical here,just dont pile on so much that it is more than 3/4 of an inch high,or it wont dry very well). Bake the MgSO4 for 2-3 hours(3 is a better number since its always dry by then), remove and let cool for 10 or 15 minutes. Once cooled, pick up a clump and grind it in your fingers, it should crumble to fine/dry/bright white dust(it looks like plaster dust at this point, bright but still flat white, not twinkilie or sparklelie like it is fresh from the carton), this dust should kick up into the air easily, with little wind, just the act of pouring it into a storage container should kick up a good little bit. If your MgSO4 dust behaves like I just described, its good to go. Oh yeah, he MgSO4 will usually bake into semi good sized plates(1-4 inches in diameter), it crumbles very easily, you dont even need a mortar and pestil(Iuse a DRY! blender for mine, but I have also just putthem into thick zip-lock bags and hit it with a rolling pin,ect). Just make sure its pretty well ground-up, so you expose as much surface area as possibleto the solvent. There you have it guys, a cheap, safe and easy way to produce your own dry extraction solvents, from non-watched/suspicious items(hope someone uses this **** because, its really useful for the home/kitchen chemist).

Preperation of dry solvent: I decided to use acetone for my first solvent extraction. I bought a gallon on the way home this morning at wall-mart, only ran me about ten bucks. A gallon is 8-10 times more than you will ever need but, compared to the quart for 6 bucks you cant beat the price break. Plus, Acetone is also a good the solvent for cleaning lab glass,some plastics,metal parts,and almost everything else in you lab. Acetone(and distilled water for that matter) has always had a corner stone in professional labs as well as colleges, you just cant beat it. Pour what ever amount of solvent you need, plus an extra 30% into a container(plastic,glass,metal, its all the same at this stage)of suitable size,do try to leave yourself some head room though. Dump in 2-3 grams(if you dont have a scale just add MgSO4 to the point where its volume is about1/6-1/5 the size of the total volume of solvent being used) of dry MgSO4 for every 50mls of solvent in the beaker. Agitate it real good for a minute or two(a water bottle with a screw cap is an old ghetto favorite,very reliable,and you can shake your *** off and not worry about spilling,sloshing,and re-absorbing atmospheric moisture), set the beaker aside and let the MgSO4 settle to the bottom(mine usually takes an hour or so to settle completely. After settling, decant(pour off) the solvent from the MgSO4, you cant get all of it without getting some of the salts so dont bother. Pour off as much as you can easily,when you see the salts rushing towards the lip of the beaker, just stop(remember we added that extra 30% to acount for losses along the way). Whatever anybody does never try to just filter them out, they are to fine of particles, and go right through coffee filters,and most lab grade filters as well(except the really fine ones).We now have solvent thats dry enough for our purposes. This process can be applied to most common organic solvents(and all of the ones we use except Ethanol, all other alcohols are okay though). Just remember. store what you dont use(dry solvents and dry epsom salt) in an airtight container, so as not to re-absorb moisture from the air.

I had never made a Dewar condenser before, but it was pretty easy. I bought a stainless steel thermos from wall-mart, its maybe a little taller than a foot and it holds about a quart of liquid, more than big enough for me. Two holes were drilled into the thermos,both through the side of it, into the vaccuum wall(to be clear: one at top, one at bottom, through the outer wall,NOT BOTH WALLS!). Drilling these two holes is not easy to do, the first was done with a diamond tipped hand drill. I eventually got it through but man, it kept slipping when you apply pressure to the drill to start the hole. Looking back, securing it in a vise would have made it alot easier than trying to fight it out with the damn thing. My second hole was done on a drill press at work and worked marvelously. The Thermos should now have two holes in any position that allows the space between the inner and outer wall(what use to be the vaccuum) to fill with liquid when submereged upto within a few inches of the top. At this point its easy to figure out how this fancy sounding piece of equipment works to condense and store liquid Butane for a little while. Only thing that sucks is that this is really all you can do with this piece of equipment. Its kinda worthless if your not making hash.

Well thats all the prep, lets get to the fun stuff.

THE FIRST EXTRACT: Into a one-liter, round, flat-bottomed flask(24/40) was placed 14 grams of kind bud trimmings and leaf trimmings(ground in the blender),500mls of dry acetone,a magnetic stir bar,and fitted with an 18 inch allihn condensor, and placed on a mag stirrer/hotplate combo, the rig was also secured in a ring stand. Stirring has been started,and is upto the highest setting possible without it missing. I started the reflux maybe an hour ago so, we got some time to wait till my next post on my progress. I want to boil for at least 24 hours,since I feel this extraction is the most important(wanna get all those goodies out). Once its done, Ill sepperate out the solvent and extract the plant matter again with 250mls of Acetone this time, I will then combine all extracts and strip-em together.

Well guys, thats all I got for now, till Im done refluxing anyway. If theres any questions anybody needs answered or clarified, Ill be happy to try to help and explain.

I could not have done this without MPs help, thanks for keeping me motivated guys(especially you Stoney), now I need a nap pretty damn bad.

Good morning guys, Ill catch ya'll later tonight.
Prometheus
 

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