Isomerization CBN > THC with H2SO4

OK, if it isn't already obvious, this thread is for people with a background in organic chemistry.

Below is a technique that is said to convert CBN to THC and to convert some forms of THC into more powerful forms.

The technique has been floating around for a while and appears in at least a couple of books. Do you think this information is credible? Although I could certainly follow these instructions, I'm not good enough with reactions to know if this is bunk or not. Any opinions?

Plus, even if it is correct, is there really a need to go to all this trouble given the potency of todays weed?

Isomerization: This method is out of "Dr. Atomic's Marijuana
Multiplier," one of those early 70's doper pamphlets. This process
assumes you have pure hash oil to begin with.

"Dissolve the hash oil in absolute ethanol or pure methanol in the ratio
of one gram extract to ten grams solvent. There must be no water in
this solution, as the next step is the addition of one drop of 100%
sulfuric acid per gram of extract. Add the acid slowly, drop by drop,
stirring slowly and completely, with a long glass stirring rod. Place a
Pyrex pot containing the extract-alcohol-acid solution into the
refluxing apparatus and reflux for two hours. The acid will not
evaporate and will remain in the Pyrex pot. Allow to cool. Take the
cooled solution, pour with an equal volume of water and 1/2 volume of
petroleum ether into the ether-extraction apparatus (separation funnel).
Allow to settle, and drain the ether extract layer. This leaves an
ether-extract-acid mix from which the acid must be purged. To
accomplish this, pour the ether-extract-solution into four volumes of 5%
sodium bicarbonate solution (1 gram bicarb. in 20 grams of water). This
will neutralize the acid, releasing CO2 and leaving a solution of sodium
sulphate. Allow this to settle into layers, then drain the
ether-extract layer. Mix the ether-extract solution with an equal
volume of pure water and let it separate. Drain off the ether-extract
layer. Evaporate the ether and what remains is hash oil in which all of
the cannabinoids have been converted into THC."

Of course it's not necessary, but sounds like an interesting experiment. Try it and you tell us if it was worth it.

I'm hoping someone has tried it or is really an O-chem pro. I'd hate to source all that stuff and have it fail - or worse make someone sick. On the plus side, the proper lab equipment can be purchased cheap on line.

RW,

I'm a professional organic chemist and drug discovery scientist. I would definitely advise against this kind of "bucket" chemistry. There are a wide variety of cannabinoids and various and sundry other organic (oil) soluble compounds in a oil extract of cannabis. There are probably some cannabinoids such a cbd that could be converted to THC by treatment with methanolic acid. The compound CBN is not one of them IMO, The structure of cbn and thc are shown below. CBN is an oxidation product of THC. Acid would be unsutable to reduce the upper aryl ring of cbn (very stable).

THC Unknown side reactions also promoted by these acidic conditions can lead to unpedictible compounds with unpredictible effects. So I'd try a good cure and extraction at cold temps. Google super critical butane and be careful. If you want to get fancy buy some LH20/ sefedex and isolate the delta 9 like we did in college...thats strong suff.
HM

Damn...hes the right guy for the answer.

How exactly did you used to use Sephadex to isolate the thc?

out.
PurfectStorm

Thanks highonmt. That is exactly the kind of answer I was looking for. I had a feeling one might wind up with some unexpected substances when reacting a plethora of substances in the above manner. That is why I asked.

I would love to hear about this other extraction technique if you are so inclined.

Peace
doublejj
P.S. This stuff makes cooking crank sound safe! I'll stick to ice & water!

interested, subscribed

I would say it's not nearly as dangerous or remotely as toxic as making meth in a bathtub... performing a reaction on a mixture is just sloppy chemistry. LH20 is a media used in size exclusion chromatography. We had 8ft tall columns packed with the stuff. Solvent is passed through the column and plant extracts are loaded on the top. Quite a suprising array of pigments appear as bands moving along the column. After some spectroscopy to identify the fraction with thc in it we did a run on the hplc. My advisor would have thrown us through the window if he had known. Sure was a rewarding experiment...
Stay Safe,
HM

highonmt said:

I would say it's not nearly as dangerous or remotely as toxic as making meth in a bathtub... performing a reaction on a mixture is just sloppy chemistry. LH20 is a media used in size exclusion chromatography. We had 8ft tall columns packed with the stuff. Solvent is passed through the column and plant extracts are loaded on the top. Quite a suprising array of pigments appear as bands moving along the column. After some spectroscopy to identify the fraction with thc in it we did a run on the hplc. My advisor would have thrown us through the window if he had known. Sure was a rewarding experiment...
Stay Safe,
HM

Click to expand...

LOL, OK. So this is something that would need to be done in a university lab or the equivilent. It's not something that could be done in a makeshift lab. Obviously more trouble than it would be worth. Just thought I would ask anyway.

My latest idea is to do a bubble bag run, save my most pure product and butane extract all the less pure product that is small enough to run. The oil would be mixed with the best product from the bags.

This should give the best bang for the buck as far as dealing with trim material.

RickWhite said:

LOL, OK. So this is something that would need to be done in a university lab or the equivilent. It's not something that could be done in a makeshift lab. Obviously more trouble than it would be worth. Just thought I would ask anyway.

My latest idea is to do a bubble bag run, save my most pure product and butane extract all the less pure product that is small enough to run. The oil would be mixed with the best product from the bags.

This should give the best bang for the buck as far as dealing with trim material.

Click to expand...

Lil somethin i researched and sounded like the best/easiest method of em all if you have some extra money to throw around. Called and ISO2 isomerizer, made em in the 70s and apparently it was the only isomerizer manufactured that worked well, and alotta hippies got some fuckin decent hash off of ditchweed they found.

Apparently theyre really rare now so dont be suprised if the bids go way past 250 (even tho this one seems to be missing a couple parts)

http://cgi.ebay.com/ISO2-Essential-Oil-Extractor_W0QQitemZ230401931006QQcategoryZ101965QQcmdZViewItem

out.
PurfectStorm

RickWhite said:

LOL, OK. So this is something that would need to be done in a university lab or the equivilent. It's not something that could be done in a makeshift lab. Obviously more trouble than it would be worth. Just thought I would ask anyway.

My latest idea is to do a bubble bag run, save my most pure product and butane extract all the less pure product that is small enough to run. The oil would be mixed with the best product from the bags.

This should give the best bang for the buck as far as dealing with trim material.

Click to expand...

RW,

Yes the isolation of pure natural products requires some very specialized (read $$$$) apparatus. Thankfully I had a great reseach group. I would not worry too much about the bubble bag unless you like hash. Supercritical fluid extraction with butane is very efficient and you'll make stellar quality oil with just trimmings. As an experiment we tried smoking (yes we let the butane evaporate first) some of the trimmings to see if there were any remaining cannabinoids. It was like smoking the lawn clippings. The trimmings are still green after extraction. The oil has mainly cannabinoids no chlorophil or pigments and it whups your ass when spread on a joint. Heres a link.http://www.erowid.org/plants/cannabis/cannabis_info22.shtml
It goes without saying put out your joint before popping the butane cylinder.
HM

Well, an inexpensive moonshine still with a water condenser can be purchased on ebay for $50. Using your solvent of choice one could do a standard extraction and then purify as desired. There are various ways. But, I've seen good results come from those bubble bags and they are cheap and easy.

The question is, what is the best way of processing a grocery bag full of leaf material. Sure I could extract with Isopropyl and even purify with diethyl ether and all that jazz but what am I really gaining from a huge pile of leaves. I have seen butane extractions that worked great but it isn't suited to a huge bag of leaves. That's why I'm thinking of using the bags until my material is a manageable quantity and then using butane.

Really, when I first heard of the bags I scoffed at them but after seeing some of what they produce I am impressed. Does some resin get wasted - I'm sure. But, is that little bit worth all the distilling and what not - probably not. Now if it were bud I wanted to extract that would be different, but for trim this should be golden.

PurfectStorm said:

Lil somethin i researched and sounded like the best/easiest method of em all if you have some extra money to throw around. Called and ISO2 isomerizer, made em in the 70s and apparently it was the only isomerizer manufactured that worked well, and alotta hippies got some fuckin decent hash off of ditchweed they found.

Apparently theyre really rare now so dont be suprised if the bids go way past 250 (even tho this one seems to be missing a couple parts)

http://cgi.ebay.com/ISO2-Essential-Oil-Extractor_W0QQitemZ230401931006QQcategoryZ101965QQcmdZViewItem

out.
PurfectStorm

Click to expand...

That looks like some type of soxlet extractor. A solvent is poured in and heated to a boil at the bottom portion. There is a mesh cup at the top full of clippings and it gets continually extracted by hot liquid(heat is bad). This method is effective but much less precise. You must use organic solvents(methylene chloride is best but toxic) to avoid the presence of lots of chlorophil and the associated bad taste. Some things that were "killer" in the seventys often would not be considered great today. I fondly remeber it as years of mexican bricks in black plastic, great skiing, Black Sabbath, AC/DC...

SCFE is the caddilac of plant oil extraction. Industrial supercritical CO2 extraction plants are common. Butane has the unique property of being at it's critical temp and pressure near room temp. Additionaly it evaporates completely with some mild warming of the oil. It's a really cool experiment but do it outside and do not burn yourself up in a cloud of flaming butane... it would suck...
HM

RickWhite said:

Well, an inexpensive moonshine still with a water condenser can be purchased on ebay for $50. Using your solvent of choice one could do a standard extraction and then purify as desired. There are various ways. But, I've seen good results come from those bubble bags and they are cheap and easy.

The question is, what is the best way of processing a grocery bag full of leaf material. Sure I could extract with Isopropyl and even purify with diethyl ether and all that jazz but what am I really gaining from a huge pile of leaves. I have seen butane extractions that worked great but it isn't suited to a huge bag of leaves. That's why I'm thinking of using the bags until my material is a manageable quantity and then using butane.

Really, when I first heard of the bags I scoffed at them but after seeing some of what they produce I am impressed. Does some resin get wasted - I'm sure. But, is that little bit worth all the distilling and what not - probably not. Now if it were bud I wanted to extract that would be different, but for trim this should be golden.

Click to expand...

I think you're on the right track if you have large volumes of trim and want to only do one extraction. I have not used a bubble bucket personally but they seem to make great hash .

For butane extration use very dry trim we rubbed it on hardware cloth over a bucket to pulverise it and get rid of some of the leaf stems, then packed it into a 2ft long 2" PVC pipe extracter lined with glass. One cyclinder of camping butane. and the whole column was done. We bought a case of gaz and extracted a couple large garbage bags. Your bubble bucket idea would be cheaper in the long run. I just might invest in one...Cheers
HM

RickWhite said:

Well, an inexpensive moonshine still with a water condenser can be purchased on ebay for $50. Using your solvent of choice one could do a standard extraction and then purify as desired. There are various ways. But, I've seen good results come from those bubble bags and they are cheap and easy.

The question is, what is the best way of processing a grocery bag full of leaf material. Sure I could extract with Isopropyl and even purify with diethyl ether and all that jazz but what am I really gaining from a huge pile of leaves. I have seen butane extractions that worked great but it isn't suited to a huge bag of leaves. That's why I'm thinking of using the bags until my material is a manageable quantity and then using butane.

Really, when I first heard of the bags I scoffed at them but after seeing some of what they produce I am impressed. Does some resin get wasted - I'm sure. But, is that little bit worth all the distilling and what not - probably not. Now if it were bud I wanted to extract that would be different, but for trim this should be golden.

Click to expand...

I'm in the same boat with tons of leaf... I was advised to try the same thing I made my hash then take the hash and make honey oil and mix back in some of the unpressed hash (kief) before heating and bricking it into bubble hash.

Let me know how that works out, it'll be a bit before I get the butane and if you find the best ratio oil to kief or a trick that makes it easier or mistake I can avoid...

I have yet to measure the amount of powder to oil. The best way I can think of is to warm the oil to a liquid and mix in powder a bit at a time using a flat head screwdriver or the like. Once it starts to firm up you can continue working in the powder with the back of a strong table spoon or other pressing tool until it becomes a firm but pliable chunk.

Now if the end product is mostly trichome heads this might change the dynamic, but I suspect there is a good amount of plant matter. I look at adding powder to the oil simply to make it easier to handle and use. The weight gained by doing this is negligible.

Well I did some more research into this "isomerization" of thc. In reality the reaction you mentioned in the first post is an acid catalyzed cyclization of cannabidiol cbd


to THC

Just google "acid catalyzed dehydration of cbd" So if you have some herb high in cbd you can definitly increase the thc content of the extract; but any other acid catalysed reactions which are possible in the mixture will happen as well. Interesting stuff.
HM

highonmt said:

Well I did some more research into this "isomerization" of thc. In reality the reaction you mentioned in the first post is an acid catalyzed cyclization of cannabidiol cbd

to THC

Just google "acid catalyzed dehydration of cbd" So if you have some herb high in cbd you can definitly increase the thc content of the extract; but any other acid catalysed reactions which are possible in the mixture will happen as well. Interesting stuff.
HM

Click to expand...

Can we be sure that the THC doesn't undergo any change? Also, if we wind up with God knows what, could any of these substances be harmful?

RickWhite said:

Can we be sure that the THC doesn't undergo any change? Also, if we wind up with God knows what, could any of these substances be harmful?

Click to expand...

The THC should be stable to these acidic conditions. As for other compounds; who knows what else could happen. It is impossible to tell without careful analysis. I'd just stick with a good modern high thc strain.
Good luck
HM