Author Topic: p2np reduction failing on me (Read 755 times)

T-cowboy · « **on:** August 14, 2012, 11:01:04 PM »

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http://en.wikipedia.org/wiki/Phenyl-2-nitropropene

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i could not resist posting a new topic, as i have wasted some good p2np.

Anyways:

i took 100ml of 80% acetic acid, put in 7-8 gr alu foil that was ripped, without wrinkling it.

dumped in 350 mg Hg nitric salt, waited until the solution was a tiny bit grey..

in the mean time i tried to dissolve approx 5 gram p2np in 50ml IPA with heat.

This got dumped in the Acoh solution, and i waited for the solution to turn violent.

it did get hotter, and blacker, but it was a very mild reaction.

after a few minutes the hydrogen evovling reaction started to slow down. also the temp.

So i prepared a naoh solution, and put this in slowly. ( very vigorous) until phase seperation.

this resulted in a small layer, that was clear but only ipa smell was present.

Then i tried putting in xylene for extraction that resulted in a milky layer that was impossible to seperate.

Any help or advice would be nice.

Thanks in advance

Electro´S · « **Reply #1 on:** August 15, 2012, 10:04:19 AM »

Hi Cowboy.

Firstly you nitric salt maybe work or maybee not... This is not mild exothermic reaction, this one runs likes a Volcano eruption or a Rocket launcher, you know?.
And in the other hand you don't separate the organics, so you can said if was success or not, simply you had no finish your work.
Anyways i can say you than if you grind your aluminium as much as you can (like a powder) the reaction will be more energetic (exactly in the way than this reduction needs) and the second recommendation is vaccum filter the sludge two times washing the sludge in the filter with a little bit of distilled water to recover something of the acetate salt remained in it.
Them neutralization and extraction step is like a child game.
And your mercury will not be present at all in your extraction step.
And the vest part is than Dry sludge is more easy and safe to dispose properly than litters of liiquid mercurated stuff.

Electro´S · « **Reply #2 on:** August 15, 2012, 10:10:00 AM »

Oh Sorry... Add more Solvent, heat the mix, Stirr it slow with a glass rod, add Enough Brine...
Come on!!!! It's time to fight the emulsion!!!

POSEIDON · « **Reply #3 on:** August 16, 2012, 01:06:05 AM »

look this pdf

carl_nnabis · « **Reply #4 on:** August 16, 2012, 02:09:53 PM »

you have to probably dry the xylene after separation with a drying agent, also you have to bee more patient, heat the reaction as it wont kick off, iin this small scale, best reflux an hour and let it cool down completely, then add cold lye.
the reaction is over when the Al has completely dissolved.
have a bucket full of cold water at hands if you experience your reaction vessel is too small.
how large was the one used?

antibody2 · « **Reply #5 on:** August 16, 2012, 04:13:46 PM »

If you got a vigorous rxn when adding the NaOH, then good chance your Al had not finished reacting. This RXN needs to running full blast as others have mentioned, kick start if necessary.

Gypsy · « **Reply #6 on:** August 17, 2012, 06:37:41 AM »

my suggestions:
Use MeOH. It has a lower boiling point and requires less energy to maintain it at the right level. The lower point will also result in little to none being left once the reduction is finished. should be a nice thick cement like sludge. maybe even hard. both IPA and MeOH are miscible with xylene. So, that said Im not sure as to what you mean by a layer that was impossible to seperate. Was it an emulsion? Or was it a single homogeneous layer? Use a nice concentrated solution of ice cold NaOH. I've been using a 50% solution. No emulsions formed.
and again, try not to cool your vessel down. So make sure you have more than enough headroom. I've found during the reduction the foam produced can consume as much as 7x its initial volume.
At the this point Im not even removing the sludge. basify, and extract directly with toluene. A/B workup with a saline wash.

fishinabottle · « **Reply #7 on:** September 14, 2012, 09:20:03 AM »

Do the amalgamation BEFORE adding the acetic acid in water/IPA, say Al into IPA/water, add your mercury salt and let amalgamate very well, then add 70% acetic acid (to strong will kill the reaction), wait until the Al gets reacting again and then add P2NP dissolved in IPA/acetic acid.
Wait a little and it will get really going whats good.
Heat for half an hour after this finished and filter off unreacted Al with a metal sieve* before adding NaOH dissolved in water 50/50 (weight). I cannot see any advantage in reacting excess Al with NaOH in the end and there IS unreacted Al as a good excess is used here.
The upper layer is IPA with goodies, separate**, add H2SO4 in IPA 1 to 5 vol. (not much needed here, use a syringe and the goodies crash out***. Filter. Recrystallize or better do a second A/B/A. Done. Enjoy.
Don forget to take selene supplements to protect your dopamine receptors.

* the filtered Al will start fizzling and even burn on air so be careful and dump it quickly into water
** you can do a second extraction with an organic solvent or even fresh IPA here
*** solubility of amphetamine-sulfate is so low in this alc/water mix that drying is negelctable

More efforts are better invested in a proper recrystallisation or as said even better in basifying the sulfate/extract with organic solvent/dry this extract with MgSO4/form salt again (whats much less tedious as it sounds). This will vastly improve quality.

/ORG

Balkan Bonehead · « **Reply #8 on:** September 14, 2012, 04:18:22 PM »

Quote from: fishinabottle on September 14, 2012, 09:20:03 AM

Don forget to take selene supplements to protect your dopamine receptors.

Pardon, but what are selene supplements?

fishinabottle · « **Reply #9 on:** September 16, 2012, 11:50:56 AM »

Selen is a chemical element and the most suited antioxidant to counter methamphetamines neurotoxity.

In short: Take selen supplements from the healthstore, not ery expensive btw., and your dopamine receptors will survive, otherwise the meth will kill them over time and that is the main problem with this drug.

See attached article, many more are out there....

This is IMHO the most important point regarding harm-reduction with meth and I cannot understand why this is not pushed into the tweakers heads over and over again. Makes coming down a breeze, counters the urge for compulsive redosing and reduces the depression when stopping use after a prolonged time of consumption to almost nothing

/ORG

4studiesonly · « **Reply #10 on:** September 16, 2012, 12:17:57 PM »

Quote from: fishinabottle on September 16, 2012, 11:50:56 AM

Selen is a chemical element and the most suited antioxidant to counter methamphetamines neurotoxity.

In short: Take selen supplements from the healthstore, not ery expensive btw., and your dopamine receptors will survive, otherwise the meth will kill them over time and that is the main problem with this drug.

See attached article, many more are out there....

This is IMHO the most important point regarding harm-reduction with meth and I cannot understand why this is not pushed into the tweakers heads over and over again. Makes coming down a breeze, counters the urge for compulsive redosing and reduces the depression when stopping use after a prolonged time of consumption to almost nothing

/ORG

This is great info, so thank you....
I just glanced at the pdf just now and i wonder if this (selen) also would help the dopamine receptors when taking other drugs that injure them, in my case I'm wondering specific when taking heroin?
I have not done heroin in 11 years now, but still have problems with with feeling happines for little things like a sunny day and such things. Depressions and shit has in a way made me handicapped and fucked up my universitystudies and my worklife, last year i decide this cant go on and contacted doctors psychiatrists and soon i think they will put me on dex-amphetaminsulphate. But from time to time one also want to have a private party with other opiods, meth, mdma....

So is this selen supplement apliable to other drugs to in reducing the harm for my surviving dopamine receptors?

lugh · « **Reply #11 on:** September 16, 2012, 05:37:15 PM »

It's important for many reasons:

Antioxidants & Redox Signaling. April 1, 2011, 14(7): 1337-1383. doi:10.1089/ars.2010.3275.
Selenium in human health and disease.
Fairweather-Tait SJ, Bao Y, Broadley MR, Collings R, Ford D, Hesketh JE, Hurst R.Susan J. Fairweather-Tait, Yongping Bao, Martin R. Broadley, Rachel Collings, Dianne Ford, John E. Hesketh, and Rachel Hurst.

School of Medicine, Health Policy and Practice, University of East Anglia, Norwich, Norfolk, United Kingdom. s.fairweather-tait@uea.ac.uk

This review covers current knowledge of selenium in the environment, dietary intakes, metabolism and status, functions in the body, thyroid hormone metabolism, antioxidant defense systems and oxidative metabolism, and the immune system. Selenium toxicity and links between deficiency and Keshan disease and Kashin-Beck disease are described. The relationships between selenium intake/status and various health outcomes, in particular gastrointestinal and prostate cancer, cardiovascular disease, diabetes, and male fertility, are reviewed, and recent developments in genetics of selenoproteins are outlined. The rationale behind current dietary reference intakes of selenium is explained, and examples of differences between countries and/or expert bodies are given. Throughout the review, gaps in knowledge and research requirements are identified. More research is needed to improve our understanding of selenium metabolism and requirements for optimal health. Functions of the majority of the selenoproteins await characterization, the mechanism of absorption has yet to be identified, measures of status need to be developed, and effects of genotype on metabolism require further investigation. The relationships between selenium intake/status and health, or risk of disease, are complex but require elucidation to inform clinical practice, to refine dietary recommendations, and to develop effective public health policies.

ppanik · « **Reply #12 on:** September 26, 2012, 06:59:44 AM »

First,

Hello Vespiary ! Iam new in this forum. And sorry for my bad english.
I did not want to open a separate topic.

but i have question too.
After this reaction, when i have collected the freebase (transparent, little little bit yellow liquid),
i can see some white spicular crystals in the freebase, after a while they settle on the ground.

it is not a amphetamine salt (ph +12 is the liquid)
What is this ? And what is the mistake (i hope you know directly what i mean, when not i make a own topic in some days)

and a last question. Is it possible that i can clean the freebase like this --->
Salting the freebase with ipa+HCL. Then put the amphetamin HCL again in his freebase form (sodium hydroxide solution).
then collect the freebase and salting again with ipa+ sulfuric acid ??

thank you very much. Best regards

ppanik · « **Reply #13 on:** September 27, 2012, 09:12:47 AM »

::EDIT::
sorry for my stupidness ...

Quote

More efforts are better invested in a proper recrystallisation or as said even better in basifying the sulfate/extract with organic solvent/dry this extract with MgSO4/form salt again (whats much less tedious as it sounds). This will vastly improve quality.

thx

But my other question is still unanswered. What is this spicular crystals in the freebase after separate from the sludge?
Sometimes the sludge polymerizes, what is going on there ? The upper layer is normal but the sludge turns into a gel/polymer (what ever)

best regards

no_dream · « **Reply #14 on:** September 27, 2012, 05:48:01 PM »

1. Use amalgamated Al in alcohol and slowly add nitro dissolved in acetic.

2. Dissolve the base in DCM, wash with water, brine and extract into HCl. Wash with dcm, basify, extract with toluene

3. Strip the toluene and vacuum DISTILL the base!

ppanik · « **Reply #15 on:** September 28, 2012, 06:59:31 AM »

ok thank you.

1. last times i threw all nitro at once into the amalgamated Al + IPA + acetic. Slowly is better !? right ?

2. can i used for the DCM ---> Benzinum medicinale (petrolether) ?

3. what temperature is needed for vacum distillation the base ?

THANK YOU

Gypsy · « **Reply #16 on:** September 28, 2012, 03:07:53 PM »

Quicker is better.
http://127.0.0.1/talk/index.php/topic,2962.msg32646.html#msg32646
Might be of some help to you.

T-cowboy · « **Reply #17 on:** September 28, 2012, 07:11:32 PM »

Tip of the week:

When the orange like ipa is seperated (twice collect) pour in half amount of COLD anhydrous acetone, then drop by drop pour in sulphuric acid. this ensures nice white sulfate snowing in the flask, without re-x afterwards. filter this. dry this. PH 7-6 i think.

T-cowboy · « **Reply #18 on:** September 29, 2012, 07:58:42 PM »

everybody has its own variations, variables. I am not meaning this in a negative sense at all!

My conclusion to this comes down to wich nation,country the chemist comes from. You see: EU likes Alphamethylphenethylamine US: Methylatedamps= EU p2np reduction.

IT al boils down to factors like the type of AL foil, this is different from country to country, by that i mean the type of AL foil . The type of OTC solvents, eventhough the same it can be diluted with "unknown" substances.

My own experiments are different every fudging time! with the same exact equations of solvents,substrate etc etc. even work up- before reaction.
sometimes it starts slowly and surely. wich gives the feeling of: yes this is. but not an extreme reaction.

Then other times, nothing happens. it just heats and thats it.

Then once, BAR-BAR-BAR (casino slot style ringing) reaction with the AL so extremely reacting one would think naoh was being added. rising a bit in the flask.

But then again im just a dumbass, for trying to make something scheduled by international law.

However, i have read that instead of using IPA, usage of Etoh should increase yield. I have tried this, based the reaction. added IPA to collect the Etoh also (miscible)
and i cannot tell surely if the yield was higher, but post-product really had lower potency, in comparison to IPA as started solvent for nitropropene.

Well thats it from the dumbass, have a pleasant weekend.

T-cowboy · « **Reply #19 on:** September 29, 2012, 08:00:33 PM »

Quote from: Gypsy on September 28, 2012, 03:07:53 PM

Quicker is better.
http://127.0.0.1/talk/index.php/topic,2962.msg32646.html#msg32646
Might be of some help to you.

why was there no water involved in your reaction? or did i miss something

Author Topic: p2np reduction failing on me (Read 755 times)

T-cowboy

p2np reduction failing on me

Electro´S

Re: p2np reduction failing on me

Electro´S

Re: p2np reduction failing on me

POSEIDON

Re: p2np reduction failing on me

carl_nnabis

Re: p2np reduction failing on me

antibody2

Re: p2np reduction failing on me

Gypsy

Re: p2np reduction failing on me

fishinabottle

amalgamation problem

Balkan Bonehead

Re: p2np reduction failing on me

fishinabottle

SELEN !

4studiesonly

Re: SELEN !

lugh

Re: p2np reduction failing on me

ppanik

Re: p2np reduction failing on me

ppanik

Re: p2np reduction failing on me

no_dream

Re: p2np reduction failing on me

ppanik

Re: p2np reduction failing on me

Gypsy

Re: p2np reduction failing on me

T-cowboy

Re: p2np reduction failing on me

T-cowboy

Re: p2np reduction failing on me

T-cowboy

Re: p2np reduction failing on me