Your 3 liter reactor, was that a glass(lined) one? SSteel ones can force to form a Pd layer on the walls.
Your 5% Pd/C, was that reagens grade, from a professional source, or did you make it yourself?
Most homemade Pd/C is doomed to fail.
How much GAA was needed? Do you really have to acidify? Where do you get that from?
The Toluene was separated off, and the aqueous layer, which was basified slowly with 25% NaOH. It heated up a little, but nothing dropped out.
I think you have to (re?)read MadMax sticky Newbee post about Acid/Base washes: Post 286519 (missing)
(MaDMAx: "LOOK! Recrystallization and A/B general info", Newbee Forum) :
Once you have freebase in your non-polar you can wash the non-polar solvent with water to get rid of any non-freebase drug material (such as excess lye). The water will not remove any of your freebase.
Then to recover your hydrochloride salt (the most popular form of most drugs), you react it with hydrochloric acid. Muriatic acid is hydrogen chloride (HCl) dissolved in water. So if you add this to the non-polar with the freebase, the freebase will react with the HCl to form the salt, which is now soluble in water and not in non-polar, so it will dissolve into the water layer, which you can separate and evaporate to obtain your crystals.
Etcetera.
Ofcourse nothing dropped out, you will have to acidify your basified solution again, then boil off the water. LT/
PS:
The organic layer was recovered and suspended in 200 ml of water, to this there was added 2 L of 5% HCL and shaken. The oil was not soluted
Yep, ofcourse not, you have to solute your freebase oil in a nonpolar solution, preferably dry >98% acetone IMHOpinion.
For your info:
Freebases and salts usually have drastically different properties. An important one is that freebases are usually soluble (will dissolve in) in non-polar solvents such as toluene and hot naphtha, and not soluble in polar solvents such as water. The salts are usually the opposite, soluble in water, but not toluene etc. This is how acid/base extractions (A/B) work.
You can basify your molecule with NaOH (lye) to form the freebase, which is not soluble in water, but it will dissolve in a non polar solvent. So you add your non-polar solvent and the freebase goes in to it (a lot faster if you shake it all up instead of waiting for the freebase to float up to it). Once you have freebase in your non-polar you can wash the non-polar solvent with water to get rid of any non-freebase drug material (such as excess lye). The water will not remove any of your freebase.
Your 3 liter reactor, was that a glass(lined) one?
My reactor is PP, with teflon coated stirrer, no ss here.
Thanks for the thought though.
Your 5% Pd/C, was that reagens grade, from a professional source, or did you make it yourself?
It was bought.
How much GAA was needed? Do you really have to acidify? Where do you get that from?
https://www.thevespiary.org/rhodium/Rhodium/chemistry/mdma.catalytic.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/mdma.catalytic.html)
and JM
I think you have to (re?)read MadMax sticky Newbee post about Acid/Base washes:
Actually, I did, that is why the acidic water, product and Toluene (a non polar) ended up together after a failed crystallization. This is what I said:
The organic layer was then recovered and suspended in 200 ml of water, to this there was added 2 L of 5% HCL and shaken. The oil was not soluted, 250ml of Toluene was added, and the mixture shaken vigorously.
Ofcourse nothing dropped out, you will have to acidify your basified solution again, then boil off the water.
What I was expecting to drop out is of cource not crystals, but the oil. If the product was dissolved in the Toluene, and shaken with acidic water, then that acidic aqueous layer basified, that should have made the freebase drop out. Which would have been taken up in fresh Toluene, and redistilled. Tell me I am wrong.
Here is also a quote from terbidium:
terbium
(Old P2P Cook)
05-18-03 15:31
No 433999
Then if you put the freebase in acidic water (ala BrightStar) will it dissolve?
MDMA freebase will dissolve in acidic water. If you have something that will not dissolve in acidic water then that something is not MDMA freebase.
--------------------------------------------------------------------------------
All those moments will be lost in time, like tears in rain.
From https://www.thevespiary.org/rhodium/Rhodium/chemistry/dmfo2wacker.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/dmfo2wacker.html)
"Vacuum distilled at ~2.0mm Hg to recover 311.22g PiperonylMethylKetone (MDP2P) fraction between 105-114°C."
Also, I read someone saying on this board that if you don't run this hot, you mostly get MDP1P.
But then I also read that on the new bee forum that MDP1P would not form the bisulfite adduct:
GC_MS
(Hive Addict)
05-04-03 14:22
No 431333
As I remember it, aldehydes and ketones should always be able to form bisulfite adducts, except in the case of phenones (acetophenone, benzophenone, ...). But frankly, I can't recall where I read it.
terbium
(Old P2P Cook)
05-04-03 14:50
No 431343
Propiophenone.
except in the case of phenones (acetophenone, benzophenone, ...)
Or propiophenones as in 3,4-methylenedioxypropiophenone (MDP1P). This is what Vogel seems to say.
1. We (moderators/admins) don't have and will never have (probably) a Hive research laboratorium which only dedication would be to check and recheck ALL chemistry posts in a lab.
We also obviously don't have the time personally to perform ALL reactions and posted methods around here, so we can only assist theoretically or in a few cases practically based on personal experience in rating the credibility of posts.
The rating system is implemented just a few months now, and NOBODY up till now from us Moderators has found it possible to rate older posts AFTER the rating started, because implementing our rating window in old posts would prolly wreck the whole board( or not, Admins?)
In most cases you can count however on the credibility of most methods IF they are rated or appear on Rhodiums site. And STILL there could be major(seldom) or minor(often!) flaws in it. We have NO Pfizer research labs with millions of research money at hand!
2. The same goes for Rhodiums site, just as obvious. As anyone with a birdbrain can see, the huge amount of articles in there would even make it impossible for a well equiped University lab to check/perform all articles there.
""How easy would it be to fix that dmf/o2 wacker post on Rhodium?""
He only changes info in articles after a few credible sources or himself(very unlikely btw) have confirmed a blatent fault in it, or even confirm that the whole method is crap, which leads to deleting the method. He should leave a note then, with enough info on the proposed method, so that Searchers who find that crap still somewhere on this board or elsewhere, will be warned of the uncredibility of it.
Btw, he has removed proven crap methods several times (without public notification, I think).
The simple fact that somewhere between the thousands of posts some one mentions that you need elavated temps for the DMF/O2 wacker post on Rhodium means only one thing:
The ones interested in it out of theoretical or practical interest will find it automatically while they are reading ALL chemistry posts every day, or use their brain a bit better and do a quick selective Search EVERY fuckin day on the subjects they are interested in, using the right words or data or abbreviations.
Then ONLY the practicising ones will try it out.
YOU seem to be one of the very first ones trying it out and POSTING on it. How many will do the same, but will not POST their findings? Because we have a terrible bunch of egocentrically greedy oriented egotrippers around here, so we are all dependend on just the very few who take the RISK to POST their results.
That's the only one fuckin reason I still reply to you: posting your research, however still mixed with rude insults.
You obviously think that the method you are working at now should have the full attention of ALL members plus the moderators, while you think it's the most important undergoing event on the planet these days. Let me tell you: all newsnetworks will differ in opinion with you on this. We also do, for the most part. Most members have their own little pearl of attention span at this very moment, and for them, the way you dress up your posts with unnescessairy comments, will give them the impression to deal with a selfish motherfucker who badly needs this board to get ANY result at all, but when his research ends up the VERY first time doing this method in a failure(normal procedure for most of us, FYInfo), starts spouting badmouthing to the very ones who have helped him in the very first place by collecting those methods in the Rhodium forum to use OR research and check further. It is NO guarantee at all that ANY method proposed there will work AT ALL, only AFTER you, the MEMBER, has repeated it to the letter and found out it does or doesn't work as proposed, perhaps and post your try-out. The bulk of them WILL work, btw.
Most moderators here around do read HUNDREDS of posts, sometimes ALL posts in ALL forums EVERY fuckin day, to keep up just THAT, the CREDIBILITY of this so important board for you all. We have tens of interesting RESEARCH posts to think about, every day, and try to answer them as good as we can, in many cases ending up in more workload, because the poster start PMing us, thus causing us double work. WORK means going to libraries, checking books and journals, PMing colleagues about it, talking to friends in real life, etc.
This is exactly the way SCIENCE works, post an article and WAIT for more than one confirmation of the proposed method or thoughts.
3.
But what I do not appreciate is people posting misinformation on Rhodium, and all over The-Hive, including your posts. You said this is how things work around here. It sounds like words of a provocateur to me.
If you don't understand by now, how utterly pitty that last opinion sounds, you should apply for instant banning this moment.
Or be considered by others here as the real provocateur.
Rhodium brings posts from the Hive solely on his OWN site, no one else does, and takes every time the risk to be attacked by selfish ones like you, if some theoretical error slipped through his attention or a method is just not working in practice, in part or totally. Nobody on this board can check personally all the Rhodium.ws methods, or my posts, or any posts, period!
What we try to do is leading our members to try at least the best methods for UNDERGROUND cooks like you?, who should take the safests and cheapests routes to their endproducts, and then post their eventual failures so we can discuss all to solve his problem, or post their successes so we all will be more secured in our belief in that very method.
And ofcourse lots of wouldbe chemists, cooks and plain idiots will interfere with that discussion, it's all to the eye of the beholder to sift through these words.
4. Log files: just type those words in Search, you paranoid droid. The server is NOT US based! And logfiles are WIPED thoroughly, we only use them to get rid of nasty critters who we feel want to undermine the principle of this board :
FREE WISDOM for ALL. LT/