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Author Topic: Jon's route  (Read 3445 times)

jon

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Re: Jon's route
« Reply #180 on: May 12, 2013, 03:35:42 PM »
just make some hbr in GAA and observe it you will see all the hso4 gets converted and you will notice the correct color slightly orange there will be no bromine in that mixture.
also just see te test I mentioned see bromosafrole will sit  on the top,
 if it sinks it's safrole and it turns purple.
so that test revealed bromosafrole.
why would I lie?
I might add that oxidation of hbr to bromine can only take place in aqueous solution and that at elevated temperates between 60-80 degress celcius

if you want to test me on this add some iodide salt and see if it gets reduced I can tell you there is no bromine in this system

and the salts on the bottom this is why I say don't stir because very little bromosafrole seeps into the salts even if you see layers let it sit you can pour all the goods without too much workup on the salt very little will be there this shit works if I had money I would make a pictorial I got the sassafras up the yen yang.
« Last Edit: May 13, 2013, 02:19:06 AM by jon »

no1uno

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Re: Jon's route
« Reply #181 on: May 13, 2013, 03:05:50 AM »
Quote from: carbonated on May 11, 2013, 11:53:12 PM
You brought up some valid concerns; it's too bad you decided to go off topic by attacking jon's character, which is completely irrelevant to this discussion.

Unfortunately Organikum has always been prone to get a little hyped up with the personal shit, I can't say too much because I do to, but that is in a large part because he has actually earned more respect than he is being shown, whereas others are being shown more respect than they have earned, it shits me too.
"...     "A little learning is a dang'rous thing;
    Drink deep, or taste not the Pierian spring:
    There shallow draughts intoxicate the brain,
    And drinking largely sobers us again.
..."

jon

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Re: Jon's route
« Reply #182 on: May 13, 2013, 03:16:37 AM »
organikum is genius he overthinks shit it's what geniuses do they think too much.
so he can accuse of unsuccessful runs yet I have yet to see one even with the amueters it helps gain confidence that  route really works I have used just bromo safrole and got 40-50
% this is pretty good and those cheao fire extinguishers at walmart are corrosion resistant I have done many bromo runs it takes 4-5 hours and I just use boiling water and extend the rxn time.
it yields higher at 100C just let it run 5-6 hours you will see the pressure is only 60 psi when boiling and ipa is a must I only get 20% in ethanol ipa is hindered so it's proton does not interfere I figured this out trail and error I spent time on this process and I know what I speak of.
what I do is make the iodosafrole and add it to 8 moles methylamine in ipa the concentration isn't all that important 10% works fine I always get piss yellow oil with a biting amine odors I know this shit works I would make 60 grams just playing around just for shits and giggles we rolled about 2 grams mdma freebase into a blunt and forced everyone to smoke it.
everyone fell in love
« Last Edit: May 13, 2013, 05:22:17 AM by jon »

fishinabottle

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Re: Jon's route
« Reply #183 on: May 13, 2013, 11:55:54 AM »
Whats that nonsense up to? You are the personification of a tibetian prayer mill repeating the same over and over and over and over and over and over and over and over...
Again.
Again
Again
Again
Again

Doesnt get any better though.

You suggest I should try this by mixing blablablabla....
Are you now completely mentally disembellied or what?
If you would suggest to run a fucking TLC on it, what I now suggest you do, or some of the sufferers of thismaybe?
Thats a method to find something out.
Mix mix and lookie lookie was not a scientific method to qualify the outcome of a reaction in my books.

Thats to stupid, that was too stupid from start, that will stay stupid all eternity.

But it will claim victims over and over and over....
Even if a TLC proves the non-viability.

Because of the repeating repeating repeating repeating...

I would like to ask you if you have no decency at all, but to ask a junkie about decency....
well, forget it.

I told what was to tell, now wank on, I am out.

poor performance btw.

bye
/ORG

jon

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Re: Jon's route
« Reply #184 on: May 13, 2013, 04:29:45 PM »
tlc's were done some spotted bromosafrole and a small safrole spot others were just one spot brmosafrole I didn't get the rf values

Quote
I went about this route for a good 4 months with no success producing HCL salts. I'm 80% sure that I produced bromosafrole and iodosafrole from TLC -- but the amination has confounded me relentlessly. 

pbinterger said this so the first two steps work he failed to use a trap and got naoh and water in his ipa/methylamine solution so you see it's just the difficulty in preparing dry methyl amine solutions that are the failure point

and all you do there is have a pressure equalized drop funnel a claisen adapter methylamine in the flask naoh conc in the drop funnel and line going to a trap one line in to the bottom to push errant alcohol out and one line halfway in this goes out to the receiving vessel and the line better have some ind of gas dispersion mechanism steel wool works.
the trick here is have that alcohol cold ice bath temps will get you about a 12% concentration which works.
and drop the naoh at a rate the alcohol absorbs it not all at once or your methylamine will simply bubble out so you see how that part can get a little tricky, btw your nose will tell you if methylamine is escaping and to slow you gas generation when done right there is no odor of methylamine.
'
« Last Edit: May 14, 2013, 02:23:53 AM by jon »

pbinteger

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Re: Jon's route
« Reply #185 on: May 20, 2013, 12:35:32 PM »
Yes I can confirm that this method does produce bromosafrole and iodosafrole respectively. I also know of one other member of this forum who has run TLC on bromosafrole from this route and confirmed that it works. I've talked to him at great length on XMPP about this route when I was attempting it.

Also for the novice, the h2so4 test gives some rough indication that you've had success. Bromosafrole does behave differently than safrole or isosafrole when dissolved in EtOH and dripped onto cold h2so4. It's interesting to observe the differences.

The yields vary on bromosafrole.

I always had the most trouble at achieving the correct molar excesses of CH5N in IPA -- my gassing rig was frustratingly under equipped and in reading this I certainly bubbled way too fast.

I've since upgraded my gassing rig. I gassed several hundred grams of HCL(g) into cold IPA yesterday and it worked PERFECTLY.

I think I'll try this route again in the near future and post my results.

_Pbint_
« Last Edit: May 20, 2013, 01:39:52 PM by pbinteger »

Electro´S

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Re: Jon's route
« Reply #186 on: May 21, 2013, 12:13:35 AM »
Yes man, try it again.
And one stop cork to reduce the bubbling speed would be interesting. (Remembering about pressure in the flask) 

jon

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Re: Jon's route
« Reply #187 on: May 25, 2013, 04:40:52 PM »
so we can resolve this now

jon

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Re: Jon's route
« Reply #188 on: June 03, 2013, 08:41:49 PM »
and quit knocking it it took me 6 months to get the methylamine solution just right after that I was batting 100 so let them succeed in the bromo runs and fail in the aminations

dimethylmercury

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Re: Jon's route
« Reply #189 on: June 07, 2013, 03:19:38 AM »
I definitely got iodosafrole with this route, and I believe I got MDA oil too, but now I'm having issues gassing with hcl, so I'm not 100% positive.

After gassing my IPA with ammonia, I added in my iodosafrole, shook vigorously, and it turned a bright red (is that the color it's supposed to turn?). I then left it in an ice bath for 30 mins to make sure it all reacted.

Then I poured the red IPA into a seperatory funnel and flooded with 10% NaOH solution. A golden oil fell to the bottom which I collected. I then extracted the IPA/NaOH solution with xylene (which turned a cloudly pale yellow) and added that to my golden oil.

I dripped this solution through dry MgSO4 so it became a completely clear and piss yellow.

Next I gassed that solution with HCl (using the sulfuric acid/HCl method) and at first nothing happened. After more gassing than I would have expected to be necessary the solution got much darker, almost brownish, and then what looked like white crystals started to form where the gas bubbles flowed. At first I was very excited, but then as everything settled there were no crystals  (I could have sworn there were at the start, I guess it's possible that it was just very small bubbles of oil) , but an oil layer had formed on the bottom of the flask.

I then tried to evaporate out my xylene with a water aspirator, and got some of it, but the amount of oil at the bottom also greatly diminished so I stopped. 

The last thing I did was flood with acetone in hopes that it would remove any water that could still be in there preventing crystals from falling out of solution, but that didn't work either. Now I just have the flask sitting in the freezer while I try to figure out what to do next.

The most frustrating bit is my solution is still testing positive for MDA/MDMA with a marquis test, so there's at least some safrole-related compound still in there. I just have no idea how to get it.

Can anyone help?

mztx

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Re: Jon's route
« Reply #190 on: June 10, 2013, 08:33:05 AM »
Hi dimethylmercury,

The ammonia/ISO was at least at 10% conc? And the iodo/ammonia in molar ratio was 1/15? If yes...

...I think that the problem was the amination temperature so as jon says the meam reaction must be at rt. and the ammonia one a little hotter (and maybe longer).
A red-like (burgundy) color would be normal during the reaction but the final color is piss yellow. I think that this is an incomplete reaction. Next time I would try at 40-50ºC and wait for the color change.

dimethylmercury

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Re: Jon's route
« Reply #191 on: June 10, 2013, 10:02:35 PM »
Thanks mztx

I didn't know it had to be that hot for ammonia, so that's almost definitely the issue.

Is there anything I can do to save it at this point or should I just toss this batch?
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