Amfetaminsyntese fra P2NP via Al/Hg (video)

HIGGS BOSSON

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I videosyntesen afamfetamin bruges der reagenser:
  • 10 g 1-Phenyl-2-nitropropen ( P2NP);
  • 100 ml isopropylalkohol (IPA);
  • 50 ml Glacial eddikesyre (AcOH);
  • 50 g natriumhydroxid (NaOH);
  • 12 g aluminium (i form af skiveskåret husholdningsfolie);
  • 0,1 g kviksølv(II)nitrat (Hg(NO3)2);
  • 2 ml svovlsyre (H2SO4);
  • 50 ml acetone;
  • Destilleret vand;
Udstyr og glasvarer:
  • Fladbundet kolbe 2 L;
  • Retortstativ og klemme til fastgørelse af apparatur (valgfrit);
  • Refluxkondensator;
  • Tragt;
  • Sigtefilter (køkkenkvalitet er ok);
  • Sprøjte eller pasteurpipette;
  • Papir tilpH-indikator;
  • Bægerglas (600 mL x2, 2 L, 1 L, 100 mL x2);
  • Vakuumkilde;
  • Laboratorievægt (0,1-200 g er passende);
  • Målecylindre på 1000 mL og 100 mL;
  • Koldt vandbad;
  • Glasstang og spatel;
  • Skilletragt 1 L (valgfrit);
  • Termometer af laboratoriekvalitet;
  • Buchner-kolbe og tragt;
  • Filterpapir;

7sbroyikpe

Beskrivelse af amfetaminsyntesevideo.
En opløsning af 1-phenyl-2-nitropropen 10 g i 100 ml isopropylalkohol og 50 ml eddikesyre fremstilles inden syntesestart. En aluminiumsfolie på 12 g skæres også i små stykker med en makulator til fremstilling afaluminiumsamalgam. Det kan klippes med en saks eller rives med hænderne (i handsker).

0:04-0:40 - En vandig alkaliopløsning til præparatet. Denne opløsning blev lavet på forhånd, så opløsningen har stuetemperatur ved hovedreaktionsblandingens alkaliseringstid i denne video. Alkaliniseringen udføres med en spontan opvarmning. Hvis der anvendes en frisk varm aq-alkaliopløsning, stiger temperaturen højere, og der kræves en tvungen afkøling af reaktionsmassen.

0:46-2:36 - Amalgam med kviksølvnitrat. Amalgameret aluminium reducerer
1-phenyl-2-nitropropen til amfetamin. Der udvikles en lille mængde gas under amalgamreaktionen, og der dannes et gråt bundfald. Det er vigtigt ikke at gå glip af det øjeblik, hvor aluminiumamalgamet er klar. Dette øjeblik kan bestemmes ved dannelse af et gråt bundfald og ved en øget gasudvikling. Det sker i løbet af 10-15 minutter fra reaktionsstart.

Vandet drænes uden at fjerne gaze, og det amalgamerede aluminium vaskes med to portioner koldt destilleret vand. Det er værd at være opmærksom på, at der frigøres gasbobler. Man bemærker, at boblerne er mindre, og at væskens farve er mørkere i et "korrekt" amalgam. Hvis reaktionen er voldsom, boblerne er store, og farven er lys, er amalgamet "forkert". Dette skyldes næsten helt sikkert mangel på kviksølvsalt. Vær opmærksom på, at kviksølvsalte er giftige.

2:37-4:28 - Den vigtigste del af processen er reduktion af 1-phenyl-2-nitropropen med aluminiumamalgam. Reaktionen er eksoterm og udføres med en rigelig varmeafgivelse. Det er nødvendigt at kontrollere temperaturen nøje under proceduren. Reaktionskolben afkøles i et isbad i tilfælde af overophedning. Det er tilladt at tilsætte koldt vand til kolben. Nogle gange kommer reaktionen ikke i gang, og så er det nødvendigt at varme reaktionsmassen grundigt op, og reaktionen kommer i gang (med et korrekt forberedt amalgam). Der frigives lugt af kogende alkohol og eddikesyre under reaktionen.
Allihn-refluxkondensator bruges til opsamling af dampe. Effektiviteten af Allihn-refluxkondensatoren kan øges med rindende koldt vand, som kan tilsluttes den.

5:04 - Reaktionskolben kan skylles med en lille mængde alkohol, og ureageret aluminium kan også skylles med det for at opsamle rester og øge udbyttet.

5:13 - Der bør være lidt ureageret aluminium tilbage. Du kan bestemme mængden af reageret 1-phenyl-2-nitropropen ud fra resterne.

5:16-6:13 - Alkalinisering. Reaktionen udføres med en varmeudløser. Resterne af ureageret aluminium vil desuden reagere med alkali og opvarme blandingen samt skabe biprodukter.
En adskillelse i synlige lag sker inden for 30 minutter efter alkalinisering.
pH-værdien i det øverste lag skal være 11-12.

6:18-7:23 -
Dekantering. Opsaml det øverste lag med amfetaminbase i alkohol. Det kan tørres med en lille mængde vandfrit magnesiumsulfat. Slaggen kan ekstraheres med et upolært opløsningsmiddel (ether, benzen, toluen), hvorefter opløsningsmidlet inddampes.

7:24-8:50 - Forberedelse af svovlsyreopløsningen i acetone. Denne opløsning er nødvendig for en mere jævn forsuring. Hvis der anvendes koncentreret svovlsyre, sker der en lokal oversyring af produktet. Derfor falder udbyttet.

8:51-10:53 - Forsuring af produktet og fremstilling af amfetaminsulfat. Til det øverste gule lag, som blev opsamlet i det foregående trin, tilsættes en forberedt opløsning af svovlsyre dråbevis. Der dannes saltflager for hver dråbe syreopløsning. Denne fase er meget vigtig, for det er nødvendigt at kontrollere pH-værdien nøje for at undgå oversyring. Forsuringen fortsættes
tilpH 5,5-6. Det oversurede produkt har en lyserød farve . Produktet vil blive ødelagt i tilfælde af total oversyring.

10:55-11:38 -
Amfetaminsulfatfiltrering fra opløsningsmidler i en Buchner-tragt under vakuum. Produktet kan desuden skylles med kold acetone på dette trin ved at hælde det gennem Buchner-tragten med amfetaminsulfatkagen.

11:41-12:28 - Filtrering ved hjælp af improviserede værktøjer. Ethvert tykt stof kan bruges som filter. Det resulterende produkt tørres på et varmt og tørt sted i flere timer for at fjerne resterende opløsningsmidler.
Det anbefales at opbevare det i en vakuumpakke.

Udbyttet er 60-70 %
.
 
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golab071

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Would it make sense, when producing larger quantities of the product, to use solvents like DMSO (boiling point: 189°C) or toluene (110°C) instead of IPA (82°C), and to place pieces of broken porcelain in the reactor to stabilize the reaction?
 

William Dampier

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DMSO at high temperature and the presence of acid will begin to degrade on DMS and release oxygen as an oxidizing agent. We have a strong release of hydrogen, which in the aggregate can give "explosive gas". Gently with experiments! In addition, DMSO itself is very smelly with high-temperature synthesis in the presence of many components. Try ethylacetate.
 

nofuckups

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What's the exact process of making the P2NP+IPA+GAA solution? Is it just mixing the appropriate quantity of each compound in a beaker, stirring it a bit and then letting it cool? I'm not sure why this part was skipped from the video.
 

G.Patton

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yes, exactly.
 

William Dampier

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When it has cooled by part of the P2NP can crystallize again. You can add this precipitate to the flask without dissolution or wash off an additional amount of IPA.
 
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8:51 - what's the shelf life of the clear oil after it's been separated?
 
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Hello!!

I am new to all this and would liek to give this a try and learn more

Do I need a fume hood for this?

I will have a respirator and nice gloves, is there anything else I need to watch out for?

Thank you
 

William Dampier

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The main thing is to have time to cool the reaction while this does not get out of a flask with a volcanic effect. Evaporation that you can get the main IPA is not so critical.
 

Chemdogkm

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depends on quantity of production,mostly just fumes, no open flames, dont ingest the poisonous chemicals.dont order chemicals from out of the country,they will get taken and maybe feds show up, dont talk to cops without a lawyer and dont let anyone in ur house unless they kick in the door with a warrant
 

Chemdogkm

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so i have an oily residue product,what is a good way to crystalize it?
 

golab071

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You need to use a solution of acid (phosphoric or sulfuric) in IPA. This is shown and explained in detail in the video available on the forum.
 

Chemdogkm

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After that.just takes forever to dry. So recrystalize with ethanol or xylene is what im thinkn
 

golab071

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Thank you for the previous responses.

The chemist has carried out their first (successful?) reaction and, as a result, has further questions.

The test subject, who evaluated the final product, compared it to the one commonly available on the street (according to police reports found online, its purity is usually around 10-20%).

I’d like to know whether the test subject had overly high expectations of the product, or if the inexperienced chemist might have made several mistakes during the process?

What can realistically be expected from the final product, and could further experiments significantly improve its quality?

The errors that, according to the chemist, may have affected the final product include:

• Completely skipping extraction with DCM (the chemist was prepared for it but lacked sufficient theoretical knowledge).

• Drying the product for too short a time and at too high a temperature.

Could this affect the product’s quality?

Does extraction with DCM involve adding DCM to the free base and collecting the appropriate layer? If so, are the layers clearly distinguishable, and which one (top/bottom) contains the product?

Could @G.Patton @William D. provide their input on this?
Thank you!
 

G.Patton

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Hello.
It is quite subjective, has he checked its melting point? Isomer ratio also play role in the product activity. In addition, there is direct dependence between its purity and potency.

It's hard to estimate its quality in accordance with your description. You should check its purity in laboratory (such as EnergyControl or so) and then try to find a problem. Is your product absolutely white?

this step is quite important in order to increase the reaction yield and get rid of Hg salts in final product.

It also can influence on the product quality in case of air exposure during its strong heating.

Yes, he has to add DCM to the reaction mixture stir it well and then separate layers. DCM layer is clearly be determinated by its transparency and smell.

By the way, will you sell your product here?
 

golab071

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Thank you!


No measurements were made, and the product was not 100% pure.


After adding the sodium hydroxide solution to the mixture, an oily layer separated after some time. So, should DCM be added to it after separation, or already at the stage of adding sodium hydroxide? I’m an amateur with a new hobby :) As you can see, I still have a lot to learn. I’ll follow the instructions and keep you updated on the progress. Any sale at this point is out of the question.
 

G.Patton

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>So, should DCM be added to it after separation, or already at the stage of adding sodium hydroxide?

It has to be added after NaOH aq sln addition and 5-10min stirring in order to let it reacts.
 
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Can I substitute DCM for Acetone in Amphetamine Synthesis?

Hey fellow chemists!

I'm currently working through an amphetamine synthesis protocol (thanks to Amine expert guidance) and I'm curious about substituting dichloromethane (DCM) for acetone. Specifically, I'm wondering if it's possible to use DCM as a replacement in the following steps:


  • Work-up: after extracting with DCM, could I use it again to wash the organic layer instead of acetone?
I understand that DCM is generally less polar than Acetone, so I'm worried about potential issues with solubility or contamination. Has anyone tried substituting DCM in this protocol before? Are there any specific concerns I should be aware of?

Thanks for sharing your experiences and expertise!
 
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