Chemistry Discussion Thread
- Thread starter MrEDuck
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canndo
Well-Known Member
Ok, I am somewhat confused with this mescaline extraction. I find instructions claiming that I should acidulate the water in order to salt the alkaloids while I am doing my initial reduction/boiling/ extraction. One method does not include heat at all, and has me baseify the liquid with the cactus in it and use the zylene.
What is the best method, boil the concoction and then alter the ph? alter the ph of the liquid before I add the bulk? acidify? or basefy?
The last time I did this was with peyote, dried and ground and don't recall any of this.
What is the best method, boil the concoction and then alter the ph? alter the ph of the liquid before I add the bulk? acidify? or basefy?
The last time I did this was with peyote, dried and ground and don't recall any of this.
MrEDuck
Well-Known Member
If you're not working with dried material I'd cook it in an acidic solution for an hour or two, then filter it and defat it. While you work this up cook the filtered sludge in acid (I'd do a min o three pulls) adding a little more acidity each time.
While you do this raise the pH of the defatted layer to 11.6 and extract with your np solvent. Repeat the process on each of the subsequent pulls from the acidified cacti broth. Then pool the nonpolar layers and wash 3x basic brine with a pH ~ 11.6. Then Concentrte it down a bit and salt out with your preferred method.
Edit: just to be a bit more clear I would cook the cactus down in the acidic solution. Freezing and thawing at least twice before starting on it helps break cell walls as well.
While you do this raise the pH of the defatted layer to 11.6 and extract with your np solvent. Repeat the process on each of the subsequent pulls from the acidified cacti broth. Then pool the nonpolar layers and wash 3x basic brine with a pH ~ 11.6. Then Concentrte it down a bit and salt out with your preferred method.
Edit: just to be a bit more clear I would cook the cactus down in the acidic solution. Freezing and thawing at least twice before starting on it helps break cell walls as well.
canndo
Well-Known Member
got it. Now let us talk about the pith in the middle of the woody core. I am stripping the core out because it will cause some havoc in my wife's equipment - BAAAAD idea, as it will turn this project from a 50 dollar endeavor into a $400 one in a few short minutes, should her processor come to harm. She is a very forgiving person and lets me use everything but her ceramic knives for my... er.... projects, once having ruined a le cruse pot with corn boiled dry - now THAT turned into a windy afternoon. (you know it has just come to me that we each have a very extensive set of implements - I with my vaccuum pumps and milligram scales and ultrasonic cleaners and glassware and mag stirurs and laimar hoods and she with her expenive pots and blenders and slicers and such)
Enough - one more thing, I believe you were paying attention during the harvest so many months ago, most are still fully green and have not dried, not even the test "plugs", which were about an inch or so slices - yes some are even growing sprites again after I plucked some of them last time and planted them. This stuff will not dry out in any traditional sense. I opted not to place the pieces in the oven because I think it will overload my grinder - I've lost several recently to other projects and they no longer cost 12 bucks each, let alone the volume I will have to go through - and this stuff turns pretty hard when it finally does dry. - and now I forgot my question - never mind - oh, what temperature is still safe for the final product if I were to dry in the oven?
But there is a pith inside of that core and I wonder if it has any active components. I would simply use it as well, no real harm done except that there is some real work involved in gettting it out as opposed to stripping the flesh from the outside of that core. Any ideas?
canndo
Well-Known Member
Some notes about MDMA synthesis. Let's start with Bright Star. It's a workable synth, but it does have it's faults. First would be the use of peanut oil. Get a real high temp silicone oil. No one watches them and they don't smoke and don't have a habit of splattering (200°C+ oil hurts like a mofo, or hellfire as a research advisor of mine said). Next up is the methylamine from formaldehyde and ammonia. Jesus fucking Christ do not use this procedure as written. When it gets to the point where you start pulling vacuum turn the heat off and let it cool a minimum of 50°C. Never turn vacuum on a hot distillation no matter how careful you think you are. I used to do analytical distillations when I worked in alt fuel petrochemical research. The first fraction was done at atmospheric pressure, and the. You cooled it before turning on the vacuum, at least that's what you do if you don't want to see the mother of all bbumps, ruin your distillation and make one hell of a mess.
Next what's up with using DCM as a solvent? Yuck, find a substitute. Also look into alternatives to DMF for the Wacker oxidation. That's some toxic shit. In the distillation don't use vacuum for the first fraction. Which should not be DCM because don't use halogenated organics as solvents if you can avoid it. Finally I don't care if you are Woodward himself recrystallize that shit. It was just sitting in a solution of mercury. If you don't recrystallize it and give it to another person you deserve to be shot in the genitals.
So let's look at dr Drool's synth. This also starts with Safrole and uses DCM. Apparently the Hive died because everyone got cancer (seriously halogenated organics are bad). Why would someone vacuum distill nitromethane? You're gonna lose half of it to your poor pumps oil. If something boils at <150°C do an atmospheric distillation.
OMG a ziplock bag has no place around chemicals. Rh where's the note saying don't do this. The reductive ammination looks sound. Do these guys have something against recrystallization? Does that ziplock bag give it some extra kick.
So both synths are reasonable, provided some changes are made for the sake of safety (sanity?). Except that safrole is harder to get your hands on than a pig in a lube factory. So how do we get around this? We can make it ourselves of course. Back in the late nineties bulk sassafras oil was getting more difficult to obtain. Needless to say this was a major problem for some people. Well it turns out that if you heat allylcatechol sufficiently (~250°C IIRC) it thermally rearranges to to 1-allyl-3,4dihydroxybenzene. That's a methylene bridge away from being safrole. Hydroxy groups are pretty good nucleophiles, and deprotonation only makes em better. So it turns out dihalomethanes have a use in MDMA synth. Just as reagents, not solvents. DBM or DIM (Cl is a crap leaving group) mixed with your allylcatechol and some base and wala, you have safrole.
Sorry it took me a few days to get this posted. I've felt terrible the last few days
I am just reviewing this. Hmmm.
Jp2cbxxxQC
Member
From Québec, Canada ..probably youll be able to coopérate with me in learning and legal statuses advantages I got within 2-c family non forbid in my province and so for pseudoe, e, etafedrine, ethylephrine ect.. and spot easy cooks! Ive managed to synthesize some good stuff wtih allegra-d that is fexofenadine+120 mg pseudoe that Ive growed into a solution with H2o and filtered knowing that fexo isnt water dissolvable just there the pure pseudo after a good heet quench was so cute I would cry then Im tryin with a lithium strip and NaOH attacks..that seem right with a bronze allure to my lithium and all reactions done Ive tried filtering , acétone cleaning and there im stuck at the Hcl gizmo thing.....I use hcl 20% with Salt (Big salt NaCl only) to create something like ammonia I guess do I have to solubilze my e in water in first case and than with a gas gizmo introduce this in the solution? correct me I you like anybody Its for a cooperation Ive got nice hints to give ! Could you give me one here
JP!!
JP!!
Hey, just read through this thread and it was pretty interesting. You guys definitely seem to know what you're talking about.
Anyway, SWIM is interested in extracting morphine from poppy straw. Most methods SWIM has run into on the internet seem to just be variations of each other, and while SWIM has used the standard method and had it work the yield was pretty disappointing.
Today I ran into this method- have any thoughts on it?
"If I had to pull morphine from pods, I would go brute force, STB: add ground pods to an equal volume 5M soln of NaOH, let soak for 4-5 hours, filter, allow microparticulate to settle, decant, then add enough CO2 to get the pH below 6 for a defat with heptane. Last step would be to slow-vap the water off under light heat to leave a goo consisting of morphine bicarbonate and sodium bicarbonate. The morphine should dissolve in ethanol, while the baking soda should not, the ethanol could then be evap'd to yield the crude.
Going with an STB route would ensure that no alkaloid remains stuck in the plant matter. Also minimizes the exposure to acid, which degrades morphine really quickly."
(source)
Anyway, SWIM is interested in extracting morphine from poppy straw. Most methods SWIM has run into on the internet seem to just be variations of each other, and while SWIM has used the standard method and had it work the yield was pretty disappointing.
Today I ran into this method- have any thoughts on it?
"If I had to pull morphine from pods, I would go brute force, STB: add ground pods to an equal volume 5M soln of NaOH, let soak for 4-5 hours, filter, allow microparticulate to settle, decant, then add enough CO2 to get the pH below 6 for a defat with heptane. Last step would be to slow-vap the water off under light heat to leave a goo consisting of morphine bicarbonate and sodium bicarbonate. The morphine should dissolve in ethanol, while the baking soda should not, the ethanol could then be evap'd to yield the crude.
Going with an STB route would ensure that no alkaloid remains stuck in the plant matter. Also minimizes the exposure to acid, which degrades morphine really quickly."
(source)
cannabineer
Ursus marijanus
I believe you need slaked lime on that, and they still work with boiled opium. Iirc. cn
yeah, that's the way swim has done it in the past, but the yeilds are very low.
Sorry to monopolize the thread, but since no one else is asking questions now anyway...
How about the first procedure outlined here? If it worked it would be really nice in that it has a high yield and doesn't require boron tribromide which is a pain to get your hands on (and even worse if it were to get on your hands
)
How about the first procedure outlined here? If it worked it would be really nice in that it has a high yield and doesn't require boron tribromide which is a pain to get your hands on (and even worse if it were to get on your hands
)
sonar
Well-Known Member
Interesting. Can you describe this in a bit more detail Duck. Would this process work with just the seeds?
sonar
Well-Known Member
Haven't we all.
