Author Topic: Peracetic in DCM - dreams of success  (Read 8699 times)

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goiterjoe

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Re: Peracetic in DCM - dreams of success
« Reply #20 on: January 19, 2002, 03:27:00 AM »
we're listening, but you haven't convinced us yet that you actually made anything yet.  I hope that you have in fact made what you claimed to, because I've been wonderinng if this reaction works for quite some time now, considering I think I was the first person here to ever attempt it(although I never finished it).  good luck man, and be sure to report back your findings.

If Pacman had influenced us, we'd run around dark rooms eating pills and listen to repetitive music

Antoncho

  • Guest
Re: Peracetic in DCM - dreams of success
« Reply #21 on: January 19, 2002, 06:12:00 AM »
But, oh, dear Chromic, of course we are all ears and awaiting impatiently the development of the events. Honestly, i find your work awesome!

Antoncho

Chromic

  • Guest
Re: Peracetic in DCM - dreams of success
« Reply #22 on: January 19, 2002, 09:36:00 AM »
I guess it's little more than the musing of a poor soul slopping together some chemicals in hopes to create something... but hey, play along. I still do not understand why the sulfate and hydrochloride salt "oiled out". Can anyone answer that? I realize it wasn't gassed... but I just don't get it.

foxy2

  • Guest
Re: Peracetic in DCM - dreams of success
« Reply #23 on: January 21, 2002, 11:05:00 PM »
Chromic
As Goiter stated how do you know that you have the salt at all?
Bioassy or any other proof?


NoJailForPot

(http://www.nojailforpot.com/)

Chromic

  • Guest
Re: Peracetic in DCM - dreams of success
« Reply #24 on: January 22, 2002, 06:57:00 AM »
The only evidence I have is that it was carried through by an acid/base extraction, and that it liberated hydrogen chloride gas upon adding conc sulfuric acid. It is, without one doubt in my mind, an amine hydrochloride salt. What other amine hydrochloride salt could it be other than TMMA-2.HCl? Can you suggest any sort of qualitative testing that I could do?

Btw, two bioassays at 40mg -(bumped)-> 80mg and 120mg did nothing (not unreasonable), I see no reason to take it higher..

Rhodium

  • Guest
Re: Peracetic in DCM - dreams of success
« Reply #25 on: January 22, 2002, 08:51:00 AM »
I assume both salts are very hygroscopic, and that's why they both oiled out. I see a very good reason to take the bioassaying to at least 250mg, and that is to see if there is any activity at all, the Shulgin criteria for something to be inactive is that it is less active than mescaline.

Chromic

  • Guest
TMMA-2 Bioassay
« Reply #26 on: January 27, 2002, 09:49:00 AM »
250mg TMMA-2·HCl handed out to two individuals, SWIM and SWIC. SWIC got mild nausea, infrequent rushes of anxiety, then baseline, mild audio/visual disturbances.. but a definite "something". SWIM got mild nausea, infrequent rushes of anxiety (quickly to baseline) often prompted by audio, delocalization of sounds, mild audio/visual disturbances... both experiences lasted some hours, only +/- through the whole time. The "rushes" were definitely + though, one being ++.

I can't really say if it's active or not.

PoohBear4Ever

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Re: Peracetic in DCM - dreams of success
« Reply #27 on: January 28, 2002, 06:02:00 AM »
Take two grams, then call me in the morning, mmmK?

;D ,

PB

concoct: 1) to prepare by combining raw materials; 2) to devise or fabricate

Chromic

  • Guest
Re: Peracetic in DCM - dreams of success
« Reply #28 on: March 15, 2002, 06:09:00 PM »
I watched the old man run an IR on the TMMA-2. The spectra looks right, it was definitely an aromatic amine and there certainly were no phenolic groups at the end of the day. The yields were poor, but the route is doable. Some of the "oil" was saved and it eventually spontaneously crystallized by itself if you get this "oiling out", don't worry about it.

As requested by others, I'll post my other dreams on PMA.

The old man was seen, a month ago or so, performing a Al/Hg reduction using the above prepared anethole ketoxime. 10 equiv of Al were used in a solvent of 90% EtOH at reflux (note: 10 equiv of AcOH would have really helped this low yield). So to a 100mL flask with a stir bar, 56mL 95% EtOH, 3mL H2O, 0.01g HgCl2, 3.8g Al were added, let amalgamate, 2.5g anethole ketoxime. (acid should have been added in small portions every hour or so) It was slowly brought to a light reflux for a few hours. Then 100mL of 35% NaOH was added and organics extracted with toluene... worked up by washing w/Na2CO3, filtering, washing w/Na2CO3, then extracting by titrating dH2O with HCl(aq).

A 17% yield of PMA.HCl (0.4g from 2.5g ketoxime) was recovered. The PMA.HCl was clean melting, smoky burning, liberates hydrogen chloride with marquis, bitter tasting...

The bioassay confirmed somewhere around 100mg... at 35 minutes the first effects were noted, his pulse was a mere 60bpm but it felt like it was going to explode. After 45 minutes, the old man noticed a definite stimulant effect, his nasal passages cleared up, his appetite went way down, he had major jaw clenching. At 55 minutes he started to experience major stomach upset, drunken, severe dizziness, cross-eyed sort of feeling, tingly all over the body. At about 1:20 his heart was pounding feeling as if it was going to explode, yawning, had a headache... Then about about 1:40 min there was vomitting, MASSIVE MIGRAINE HEADACHE (let's hope that wasn't his brain hemorhaging... heheh... shh... let's NOT think about it, m'kay?). Definite serotonin syndrome, not fun. At about 2:00 he was coming way down, at 3:30 it was over with an "afterglow" feeling.

If you haven't tried PMA, consider yourself lucky.

bicepules

  • Guest
Re: Peracetic in DCM - dreams of success
« Reply #29 on: March 16, 2002, 02:56:00 AM »

     Sounds like a fantastic experience.  Going for martyrdom?  ;D

"No I'll tell you what insanity is, insanity is majority rules"

Chromic

  • Guest
dreams of MDP2P
« Reply #30 on: June 07, 2002, 05:34:00 PM »
SWIC hasn't been sleeping well. He's been having really vivid dreams of an old man stinking up the room with MDP2P. He can't shake that smell out of his head even upon awakening. The same dude seemed to get 36.1g (60% yield) of light yellow MDP2P from 51.8g isosafrole. The funny thing is, I saw him distill the MDP2P  with magnetic stirring but ... WITHOUT A VACUUM ... and it came over at 278-288C, with the majority of it at ~284C.

60% yield of MDP2P using the peracetic after purifing by atmospheric distillation? Fuck yeah! I bet that old man is happy. I bet anyone else who uses this procedure, and purifies the mdp2p with a vacuum could perhaps see yields around 70%.

This time around he used:

Making isosafrole glycol:
51.8g isosafrole, 480ml DCM, 19.5g NaHCO3. Stir bar. Stirring in a cold water bath (no ice). Then added 191.4g peracetic acid (96.7g 35% H2O2, 92.8g HOAc, 1.9g H2SO4 -- sat 7 DAYS... MAKE SURE OF THIS! Your yields will SUCK if you let it sit any less than 4-5 days). Ran 5hrs. Added 320ml 5% NaOH to flask. Stirred. Moved to sep funnel. Drained DCM back into empty flask, dumped aqueous from sep funnel. Added 320ml 5% NaOH to flask. Stirred. Moved to sep funnel. Kept DCM. Distilled off DCM.

Making isosafrole ketone (mdp2p):
Rearranged with 15% H2SO4 w/MeOH for 2hrs. (80ml MeOH, 385g 15% H2SO4, standard extractions & washes) Then proceeded to distill.

If anyone wants more details, SWIC usually sees the man every once and a while in SWIC's sleep and SWIC will do a formal writeup.

Much thanx goes out to RoundBottom for his technique on making isosafrole.  :)  (ie 2x freeze purification, vacuum reflux for a bit, no vac heat/stir, then vac distill.. high quality iso is very easily made this way)

Antoncho

  • Guest
Ah!
« Reply #31 on: June 07, 2002, 07:45:00 PM »
Chromic!

Very cool! :)

Thanx a lot :)

Really have nothing to add, i immediately saved your post on my HD and i'll bee waiting for the more detailed description!



Sincerely,


Antoncho

Rhodium

  • Guest
Chromic: If you do an extended writeup, You'll ...
« Reply #32 on: June 08, 2002, 12:53:00 AM »
Chromic: If you do an extended writeup, You'll end up in my Peracid Oxidation FAQ...

Chromic

  • Guest
Aminates very well!
« Reply #33 on: June 09, 2002, 03:59:00 AM »
The MDP2P was aminated in a similar fashion to the PMP2P and 21.8g MDMA.HCl arose from 23.6g of MDP2P. Plus there's still some (~.5g) crystals stuck to the beaker. It was awesome processing all that ketone comfortably in a 500ml flask. The yield was 72+% from the amination (updated MeAm Al/Hg).

Btw, there is some questions of what to do if you ever see a tar form if you extract with acidic water (instead of gassing). Previously I've said that putting it in the freezer doesn't work, well, it doesn't. But do it anyways, then take a glass rod and scratch side-to-side. Eventually it will form a seed crystal and the holy ball of clear tar will crystalize into nice white crystals. (repeating another A/B will not clear up the tar problem, btw) Alternatively, you can throw a couple of MDMA seed crystals in the tar and it should crystallize that way (or leave it in a dessicator for a week, and it should self-crystallize)

PS. I scrapped away at that beaker for a while.. I'm now up to 23.6g of MDMA... 78+% yield. There's STILL some left in there, but maybe just 200mg or so... not really worth going after as it took about 10-15 minutes to scrap out that 1.8g...

Rhodium

  • Guest
Distill your freebases!
« Reply #34 on: June 09, 2002, 04:29:00 AM »
Are you really encouraging people to skip vacuum distillation of their frerbases? It is of course possible to do without and still get crystals, but just think of how much more pure the product will be - right now every amine (and some other stuff) in the solution will end up in the product, not just the MDMA. I believe that it is worth it going from <95% purity to >99% purity.

Chromic

  • Guest
Well, perhaps.
« Reply #35 on: June 09, 2002, 04:48:00 AM »
The crystals look clean and I'm happy with them. They turn purple-black instantly bubbling HCl when exposed to marquis, taste bitter, fully dissolve into water, have no strong odour and burn cleanly. I'm sure my labrats will love to bioassay this powder for me.

I want to add that vacuum distillation of the freebase, at this time, is not an option for me. Also note that Bright Star, although he includes an A/B, doesn't distill either. And in the MM synthesis there is neither an A/B nor a freebase distillation.

I would not recommend to anyone to skip steps, but these posts show that it's possible to get good quality MDMA from OTC products in high yields. That's something the Oxone procedure never did for me. If possible, vacuum fractional distillation of the ketone would have been preferred over a simple distillation without a vacuum. And sure, vacuum fractional distillation of the freebase would have been preferred over not doing it if I had a high quality vacuum and a large enough amount of freebase to justify it.

Rhodium

  • Guest
Distill or Recrystallize!
« Reply #36 on: June 09, 2002, 07:49:00 AM »
I must edit the MethylMan document immediately - performing an A/B is essential!

Yes, there are writeups out there which skips distillation, and you may get fine white crystals, but as soon as you compare MDMA produced that way with a vacuum distilled batch with GC or HPLC, you will find a lot of things in there which are not MDMA. With your current technique you get crystals of everything that that has an amino group attached, which includes all sorts of dimers and isomers. They may not make any difference for the taste, odour, color tests, solubility or the dubious test of something "burning cleanly". Possibly they may not even affect the high, but any molecule in the product not consisting of MDMA*HCl is in the wrong place, and should have been removed in the first place, as it isn't the psychoactive product we produced to eat/give away.

Recrystallizing the MDMA*HCl (from IPA/Et2O, or Acetonitrile 7ml/g) may give comparable results as with distillation, but this step is usually also skipped.

I condemn any MDMA production not involving a final proper recrystallization of the product or a vacuum distillation of the freebase oil - only a purist would do both, but at least one of them is essential for acceptable purity!

greeter

  • Guest
I must edit the MethylMan document immediately - ...
« Reply #37 on: June 09, 2002, 07:53:00 PM »
I must edit the MethylMan document immediately - performing an A/B is essential!

Rhodium,

    I'm certainly not one to tell you your business, but I think adding the A/B steps in a procedural manner with specific amounts (e.g. add 500ml 5% HCl to ... ) to the MM Al/Hg is a fantastic idea.  I do think though that most bees will eschew the freebase distillation step because the MM procedure if followed exactly yields only 20mL or so of oil.  It has to be run many times or scaled up to produce enough oil to make distillation in larger glass (which I presume most bees have) worthwhile.  I think many bees don't have that much patience when they perceive their bottom dollar profit to be just a gassing away.  Although if freebase distillation becomes de rigueur then new bees just learning will know no other way.

    I think the MM procedure left out the A/B because Ritter in TSII says that after a few washes there is "NO MERCURY CONTAMINATION".  This may(?) be the case but as you point out there is still contamination from other sources.



A watched pot will indeed boil.

Chromic

  • Guest
Well
« Reply #38 on: June 09, 2002, 09:48:00 PM »
Well, for the purposes of the Methyl Man synthesis I think three major changes need to be made with that writeup.

1) on step 17: taking the toluene extract, then washing once with 5% NaOH. Then suction filtering, I think skipping the filtration of aluminum foil chunks is sloppy.
2) on step 19: use 5% NaOH instead of water for the washes (MDMA is thought to be soluble in water). Two more NaOH washes should be enough, followed the one brine wash
3) step 22: provide a link to labtop's directions on how to recrystallize (my favorite):
Recrystallization of *.HCl:
1. Dissolve crystals in the minimum amount of hot, boiling IPA. (10-20ml/1g)
2. If the solution is cloudy, gravity filter, wash the filter paper with hot IPA so you don't
lose any *.HCl.
3. While hot, add 3-4x ice-cold acetone. Let it sit in the freezer until it's ice-cold.
4. Suction filter, wash with tiny amount of ice-cold acetone. The result is virtually pure *.HCl

4) technical correction at end of document: no water is needed for imine formation, the reaction actually produces water

With the Entropy writeup that is attached to the MM document:

Replace his using DCM for toluene. I bet his DCM held a significant amount of MDMA.HCl as it's soluble in DCM. I've tried to gas DCM with failure (then went to extract with water, and low and behold, there's the amine hydrochloride).

And with the Bright Star write up:

1) I think it should be changed to a work up similar to the MM work-up, ie basify the aluminum foil, extract MDMA freebase with toluene
2) An equimolar amount of aq. NaOH should be added to aq. MeAm before adding to the activated foil. (this extra water does NOT hurt the yields, even though the ketone is seen floating in a layer on the bottom) In fact, I think it boosts the yields because the methylamine is now as a gas (ie as Shulgin does it!!!):
"in succession and with swirling, 60 g methylamine hydrochloride dissolved in 60 mL warm H2O, 180 mL
IPA, 145 mL 25% NaOH"
3) preparing the amalgam should consist of adding alcohol with a touch of HgCl2, stirring, then adding the foil to stir until it bubbles. Then add the mixed NaOH/MeAmCl. I hate the water wash technique. It's messy and creates more volume of mercury contaminated wastes.
4) Recrystallization of the methylamine should not be left out of that document

Rhodium

  • Guest
Chromic: Could you be a very nice bee and help me ...
« Reply #39 on: June 09, 2002, 10:30:00 PM »
Chromic: Could you be a very nice bee and help me write the actual updates (what you have written above, plus adding an acid/base extraction to the MM file, perhaps using the one from the BS file) and put them into those documents (just download them from my page, change what needs to be changed, then email me the updated html files)?