Author Topic: From poppy pods and straw to smack......  (Read 351 times)

Tsathoggua

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From poppy pods and straw to smack......
« on: July 16, 2011, 09:34:28 AM »
Okay then people....

Tsathoggua just happened to have a bag of several kilos of poppy pods and some poppy straw.

He no longer gets off fully on his pain meds, so...its time for some extracting.

The plan is, to extract repeatedly with MeOH, after the entire plant mass has been reduced to stinking pulp and slush in a blender. Evap the MeOH, depending on whats left, add water, base with bicarb or carbonate (slaked lime is usually used, but Toady has none), then follow typical precedure ala afghan farmers.

http://www.pbs.org/wgbh/pages/frontline/shows/heroin/transform/

Think MeOH extraction might be a better way to start it off?

The intended end product is a mixed alkaloid fraction, largely morphine, for the preparation of dipropionyl morphine, suitable for IV use.

Roughly, how much alkaloids (mixed) can be expected to be present and extractable per kg of pods, and how much of that would be morphine? on average, that is.
« Last Edit: July 16, 2011, 09:36:24 AM by Tsathoggua »
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Tsathoggua

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Re: From poppy pods and straw to smack......
« Reply #1 on: July 16, 2011, 01:46:34 PM »
I am aware that Ca salls are used to precipitate morphine as the phenate, can group  I metal  carbonates or bicarbonates bee used   similarly?
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Tsathoggua

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Re: From poppy pods and straw to smack......
« Reply #2 on: July 17, 2011, 05:57:31 AM »
Conversation on MSN with Vesp confirmed what I thought may bee the case, that the sodium phenate salt is almost 100% certain to be soluable in water.

Looks like Ca(OH)2 will be the base Tsathoggua requires for conversion of morphine in soluable form (in the plant it is present mainly as the meconate salt, AFAIK meconic acid is unique to the poppy family)

So, has anybee done this before? if not as far as diamorphine/dipropionylmorphine, then to the point of a pure alkaloidal fraction?

Tsathoggua is particularly interested in the cinnamoyl ester derivative. He should be able to obtain some cinnamoyl chloride for nothing, quite possibly anyway, trade companies are often willing to give out small free samples for testing and assay purposes. *Old Toady licks his eyeballs clean thoughtfully*, he assumes that perhaps out of say 10-20kg of fresh pods/semi ripened pods maybe the yield would be at best a gram or two of alkaloids? or is it likely to be quite a bit more.

Anybody have a better idea about yield potential than Toady does?

He is leaning towards something a bit quicker and possibly simpler, not that its difficult in the first place, preparing a methanolic solution of acetic acid, with a little GAA, to produce a dilute solution of AcOH, and stewing the entire lot, after first pulverising the entire plant, pods, straw, leaves, the lot, seeing as how it all contains some of the goods, using a blender. Evap off the methanol, dilute in a small quantity of dH2O, then precipitate with calcium hydroxide.

Sound good?
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jon

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Re: From poppy pods and straw to smack......
« Reply #3 on: July 17, 2011, 07:39:19 AM »
average in pods is .2% about 2 milligrams/per gram
no you can't do that.
pods have too much plant celluose and particulate matter to precipitate morphine.
methanol extraction wo'nt work.
it carries too many particulates that can't be removed by filtration.
first it's water acidic ph 3.5 to 4 and maybe some alcohol mixed in.
the temp can't go above 80C or you'll destroy your alkaliod.
once you have the water extract you can use cation exchange resin SA 2 on amberlyte.
to absorb the morphine.
this can be eluted with dil. naoh with sodium bisulfate added in trace amounts to prevent oxidation.
(high ph facilitates oxidation)
the naoh water extract can then be titrated to ph 8.5 and allowed to stand in the fridge overnight to collect the morphine base.
this is the best way to get morphine from poppy pods.


this is the reference.
Extraction of morphine from poppy capsules and its recovery by ion exchange
C. L. Mehltretter, F. B. Weakley
DIGITAL OBJECT IDENTIFIER (DOI)
10.1002/jps.3030460315
Journal of the American Pharmaceutical Association
Volume 46 Issue 3, Pages 193 - 196
Published Online: 23 Sep 2006


Abstract
An efficient method for obtaining morphine from domestically grown poppies has been developed. Morphine was completely extracted from dried poppy capsules with water-saturated isobutanol containing 0.23% ammonia. By passage of the extract through a cation exchange resin bed, practically all of the alkaloid was adsorbed. Quantitative elution of morphine from the bed was achieved with dilute aqueous alkali. Crude morphine obtained by precipitation from the neutralized and concentrated eluate could be converted to pharmaceutical grade hydrochloride without difficulty. The overall recovery of morphine was 90%.

there are quick and dirty ways to get morphine from pods.
to get a mixture of 14 alkaloids with about 70% morphine content.
with little mecanical lossed too.
but that is the best way.

Tsathoggua

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Re: From poppy pods and straw to smack......
« Reply #4 on: July 17, 2011, 06:38:42 PM »
Some of that is obviously not the case jon, although thanks (and why, why, I wonder, did I have a funny feeling you might have tried this before)

Toady isn't really in the price range of ordering ion exchange resins at the moment, and they obviously are not needed. The traditional extraction is done in bloody afghanistan by pakis who don't know jack, unless it relates to either hearding, or eating goats. There it is boiled down (albeit there is something that can be improved on by a hotplate and careful temperature control)

Then the crude opium gunk (full of particulate matter, as will be the slurry that comes out of blending the pods and straw to kingdom come) is treated with slaked lime in boiling H2O (doubt its dH2O either somehow) upon which, so I believe, it crashes organic gunk to the bottom, and a scum of morphine forms on top, which is scooped off, then treated with NH3 (aq), which gives morphine base, which is then dried in the sun, to give a brown product, suitable for shipping to whoever buys morphine base from pakis.

2mg/g, excuse me for asking a stupid, stupid question...but, I'm dyscalculic, 2mg/g that works out to 2g/kg doesn't it?
« Last Edit: July 18, 2011, 09:25:06 PM by Enkidu »
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Sol Invictus

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Re: From poppy pods and straw to smack......
« Reply #5 on: July 18, 2011, 04:45:34 AM »

 I would recommend using chloroform (or possibly other chlorinated hydrocarbons) as yr solvent and ammonia as yr base when precip'ing morphine out of the filtered acidic aqueous extract.

 It depends of if you wish to remove the small amount of codeine prior to working up the M base (that's why the calcium morphinate is formed, so that the chloroform wash will only extract the codeine and lesser trace alkaloids, without having to play the delicate selective alkaloid solubility pH crash out game. And yes Na bases (NaOH etc.) are no good with this-- super high or low pHs will totally fuck yr M (you can even smell the char when it happens), and morphine base is highly soluble in basic Na solutions.

 So short of ion exchange resins (which are actually not so expensive, reuseable, and have a few legit consumer uses and are thus semi-'OTC') it's either use the calcium morphinate process, or do the acidic aq. exrtraction, then filter, then gently concentrate (BTW I'm not convinced that temps at least up to 100 C will destroy M, based on experimental evidence and a lack of authoritative data in the literature about this-- M solutions in water are boiled all time-- it seems like this is more of a "better safe than sorry" preventative gesture that has been passed down anectdotally as a sort of rumour, please correct me if I'm mistaken), and after concentration of the aq. extract(s) use ammonia to base to around pH 9.1, M base will start to crash if sol'n isn't too dilute and more will come out after a cooling stint in the fridge. One can also "salt out" the M a little after basing w ammonia if so desired, however IMHO the gains from salting out w NaCl are negligable. After cooling for full precip'n, the solids M base xtals are filtered off and dried and made as free from water as possible.

 At this point one could probably esterify as desired, but if a purer M is wanted (for example, if one were to use it as feedstock for a hydrogenation etc.) then a recrystallization from alcohol will give quite pure product (and selective solvent re-xtal'n can remove trace codeine if desired as well). Melting point and other tests can be used to determine yr M's purity.

 Oh one more thing-- as a sufferer of chronic pain who also enjoys the effects of novel potent opioids, I too was once very fascinated by the potential of the cinnamyl esters, but from what I gathered from hours of ref reading at the uni library a simple reflux w the anhydride or alkyl chloride (ala a heroin synth) won't cut it-- most cinnamyl esterifications I read about were being done with cinnamyl bromide and sodium hydride. I would love to know if there is a way that the Na hydride could be avoided in this process.

 And, finally, as Jon has pointed out in the course of some of his experiments, the comments in the literature of "such-and-such ester is x times as potent as morphine" do not always translate into the subjective reality of the bioassay-- oftentimes these SAR potency levels in the literature are established by tests on rats (like the hot plate and tail flick test etc.) and have limited bearing on the potency (much less the more subtle subjective effects) in human subjects. Furthermore, just because something is "x times more potent than Y drug" does not mean it is as good/euphoric as an equivalent dose of drug Y. There are a lot of factors at play here and sometimes even super-potent opioids once adjusted for dose are less satisfying/effective than the comparative compound, with notable differences appearing not just in quality of subjective effect but also in adjusted dose potency, duration and pattern of intensity levels of analgesia/euphoria, side-effects, and notable differences in the effect per the route of administration-- think of oxycodone, which has almost identical bioavailability orally vs. parenternally, compared to the o-demethylated oxymorphone, which while quite a bit more potent than oxycodone when administered parenternally possesses only a 10% bioavailability when consumed orally, but gives an incomparable, rushy, dilaudid-esque 'punch' that parenternal (I.V.) oxycodone simply does not deliver.

  On that note, best of luck and be careful-- the power of chemistry is a tremendous boon to those of us who suffer from chronic pain and/or opiate habituation, as it allows us to potentially gain much more activity from any opiates we might have access to. This can be viewed as a sort of vigilante subjective harm reduction, especially if the alternative is 'street drugs' of questionable cost, potency, legal risk, and adulteration.

   Oh and have you ever thought of going from DHC to DHM via simple hydrogenation and then to the lovely dihydroheroin? It's not that much of a stretch from making di-propanoyl-M from pods, provided there is a clear-cut and viable route for extracting the pure dihydrocodeine out of yr pills.

 Oh and can I just say I am tired of this ethno-centric bullshit with regard to drug chemistry being performed by "superior Westerners" versus "dirty, scruffy, non-Western, darkie-types", i.e. "if some dirty A-rab/Paki/Mexican can do it then a superior white person (whether 'skilled in the art or not') from an 'industrialized' nation like me can easily do it-- as if ethnicity implies scientific competence (sound familiar? Remember the term "Jewish science" that the Nazis used? I suppose if some 'curry-eating, cow-worshipping dot-head' can synth LSD in backwards-assed India, then any white druggie Westerner who spent 10min on Erowid could do so easily, right?).
 This line of thought is both dubious and pejorative, and contributes nothing to understanding either the simplicity/difficulty of a given process or the discussion thereof, and degrades the caliber of this forum to the likes of Z..let with its juvenile and inane 'nigger jokes' which run rampant over there and taint any valuable bits of data that might possibly be gleaned from amongst the vast sea of chafe and horseshit...   


  Take care, be safe, stay high, and stay free!

  --Sol



Sedit

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Re: From poppy pods and straw to smack......
« Reply #6 on: July 18, 2011, 09:19:42 PM »
Yesh, very nice first post, welcome to the Vespiary Sol.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

jon

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Re: From poppy pods and straw to smack......
« Reply #7 on: July 18, 2011, 11:57:17 PM »
i have experience with the quick and dirty emphasis dirty method.
use water ph 3.5 ph 4 use vinegar. you can also throw in some ipa to enhance solubility of the alkaloids it's not an exact science most heroin is made by illiterate afghani peasants trained by russian mafia and cia agents, (no offense to sol invictus there), so it's easier than you think.
extract the pods by steeping then squeezing through knee high panty hose repeat this process.
now use a double boiler setup with a fan blowing over it to speed convection and lower the solution temp.
it should never reach 80C
so use an aluminum bowl atop a pot of boiling water with the fan blowing over it.
the temp of the solution will be about 50-60 C with the fan going full speed and the water a rolling boil.
you'll evap it down to what's called pod putty.
(suprizingly the water evaporates quickly 2 liters or so will be gone in an hour or less.)
you can then extract this with hot boiling isopropanol until the alcohol takes on no more color. (you need to mix the putty well in the ipa as it's boiling in a water bath suprizingly it works well it concetrates the poppy to 100/th of it's weight to get a black oil.
the plant oils can be rinsed off with acetone if you like.
(don't use ethanol or methanol because it keeps particulates in suspension and you'll never filter that out.)
if you let the alcohol cool the crude shit will crash out.
and you can separate this.
or you can nevermind that and evap all the alcohol off then take up into janatorial grade ammonia saturated prefferably with cacl2 to salt out the crude mixture of about 10-14 alkaloids.
this soon to be dirty smack actually has qualities that refined smack does'nt.
then you filter this there will be very little of this so mind your technique to avoid mechanical losses.
of course you set the ammonia in the fridge overnight to allow complete precipitation.
(you will notice the ammonia takes on a dark color and takes up a lot of impurities as it precipitates the crude base)
this is called glazura or glaze in polski. (this is kompot heroin)
you can acylate this directly.
acetic acid also does the job but it takes 20 hours.
do it cool around 80 C or so to avoid scorching the goods.
if you want to refine it you can evap the acid/anhydride take up in water decolorize with activated charcoal, and wash with chloroform to remove much of the color and the trace acids.
i would'nt try to neutralize the water with nac2o3 because of mechanical loss.
just evap the water off using a fan and a steam bath on a pyrex dish.
the point here is even though your dealing with say 200 grams of poppy straw the maximum amount of morphine in that straw is .35% or 700 milligrams so the less you fuss with it the less you lose.

p.s. i've injected this stuff (no burn on the veins) less than a matchhead had me passed out in a bathtub for 4 hours i did'nt notice i was in a tub of freezing water don't be fooled by this stuff it's very potent.
« Last Edit: July 19, 2011, 12:13:29 AM by jon »

Tsathoggua

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Re: From poppy pods and straw to smack......
« Reply #8 on: July 19, 2011, 02:24:56 PM »
Thank you both very much, 'ol Toad is very grateful indeed for this advice.

Toady has considered preparing dihydrodipropionylmorphine also, but, but, his intent here is for recreational use. There are indeed times where his knee gets bad enough that he does, and will use stronger opioids for pain relief.

But the purpose of this, and why he doesn't turn a few scripts worth, and he could easily do so, into much more potent analogs, is that he does not want regularly to use these high potency opioids. He has some sense (in general and of self preservation).

This is to have a few grams of something handy that is both a refreshing change from the norm, that can, and will blow a sodding great hole right through his tolerance, not for daily use, becoming a slave to the needle is not something he wants. Whilst he did just order some new injection supplies, he already had a full IV kit.

When its gone, its gone, until next poppy ripening season.

(actually the fresh supplies came today, but he already had a full kit, a large pouch of varying gauge needles, syringe types, sterilising wipes etc. The only reason he ordered it, was to get certain types of supplies that when he does use an IV injection, he prefers very short, very fine needles, and he had made use of the last amp of saline he had the last time the kit saw the light of day, sweet enough, the harm reduction oriented site he bought from sent him two free amp cracking devices designed for avoiding shards when doing it by hand...very nifty indeed :))

Sol invictus....I would hardly say referring to the calcium phenate process as 'ala afghan farmers' is akin to a 'nigger joke', for the process is indeed done by afghan farmers and middlemen, who most likely, do not, possess a good, solid understanding of chemistry, of the nature sufficient enough to say, come up with procedures for the creation of other things that if they decided they wanted, them (or had heard of them), it isn't the same as calling them 'fucking dumbshit paki bastards', etc. Truth be told though, it is most likely most commonly the case that the people doing this over there do not in fact possess a sophisticated chemical/biochem education. Toady is selftaught, but nevertheless, he is fairly confident that his understanding of the process is somewhat better than an afghan opium farmer.

Although, he isn't exactly fond of taliban types, his girlfriend's eldest son is in constant danger from them, serving with the marines, and, well, he is never going to be happy that people would sent bullets and roadside bombs his way.

Toady takes and already appreciated Your point, sol invictus, about the trace alkaloids, and the differences in equivalent potency between various other opioids, mouse/rat bioassays etc. etc. Of course, it will need the codeine removing, and plant proteins, as it is intended for IV, and neither pulmonary oedema due to the former, or anaphylaxis due to the latter appeal to him.
« Last Edit: July 19, 2011, 02:35:21 PM by Tsathoggua »
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jon

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Re: From poppy pods and straw to smack......
« Reply #9 on: July 20, 2011, 12:13:35 AM »
a little codiene does'nt hurt things.
to get rid of the plant proteins and particulate matter just extract it with ipa and procedd on by basing with ammonia this gets most of the impurites taken care of.
you can further refine it but when working with small amounts it's better to use less steps.

Tsathoggua

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Re: From poppy pods and straw to smack......
« Reply #10 on: July 20, 2011, 02:47:47 AM »
It does if its injected intravenously.

IVing codeine puts one at risk of pulmonary oedema. Of course its (almost always) better to use less steps, there are exceptions, but by and by you are absofuckinglutely right.

The histamine release induced by codeine makes it highly dangerous to IV, If we are talking milligrams, or micrograms no harm, no foul, and they do make a pharmaceutical grade dihydrocodeine shot, however, it is not for IV use. It is to be used IM.

A bit of a pisstake and a waste I think. I think, possibly, just maybe, I would even get judged as a druggie from the way my face would fall, if I was told I was being given an IM shot of pain relief in hospital and then they told me it was DHC. Although, possibly not as bad as the way the needle would melt at the language I might well employ :P
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Re: From poppy pods and straw to smack......
« Reply #11 on: July 23, 2011, 02:04:12 AM »
The chemists are a strange class of mortals, impelled by an almost insane impulse to seek their pleasures amid smoke and vapour, soot and flame, poisons and poverty; yet among all these evils I seem to live so sweetly that may I die if I were to change places with the Persian king.
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