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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timeandtime

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8:51 - what's the shelf life of the clear oil after it's been separated?
 

G.Patton

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Jeg kan hjælpe dig med syntese, og du kan stille mig spørgsmål om det i private beskeder.
 

Barter

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Hi Mister G Patton , after the Aluminum Amalgated with mercury ,
It is said we have to make : P2np + IPa + glacial acetic acid .


Can we replace the acetic acid with Citric Acid ?
In which quantity?
 

William D.

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The usual replacement is formic acid, if it’s so easier. You can buy food vinegar the same way.
 

Eddybeaumont

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hello and thank you for this fabulous video. Is it possible to replace mercury (II) nitrate with mercury (II) chloride for amalgamation with aluminum? If so, does the quantity change? if yes in what quantity for the same proportion as in the video please? thank you in advance for your response
 

G.Patton

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Yes, it's said above and every post about amalgam production. Same molar ration, you need to recount quantity in grams.
 

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?
 

G.Patton

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The reaction is too violate and exothermic. It think, it have no sense.
 

William D.

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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.
 

Barter

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Please , ithe video shows 12grams of aluminum into a 2000ml flask .
But I wanted to go 24 grams of aluminum grit into the 2000 ml Flask
Please tell me what is ratio for all quantity of other components.

Is it 2 times more IPA ? Glacial acetic acid ? Sulfuric acid ? H2o ? Caustic soda ? And also what about the
Time for reaction ? Does time of reaction also double ? What about decantation when we double quantity for same glassware ?
( Attached the picture of 24 grams of aluminum into a 2 liter flask .)
Please respond need tour help to start
 

G.Patton

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Hi, you need bigger flask. Multiply everything twice. Time is about the same.

Start with smaller amount at first.
 
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Barter

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Mister Patton , can I replace IPA by ethanol , to dissolve P2np for the main reaction into the synthesis '

How much is equivalent of Ethanol to replace 100 ml of IPA for this synthesis
 

G.Patton

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Yes, you can. Same, I guess. You have to dissolve al P2NP.
 

William D.

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You can use various solvents, we even synthesized in ethyl acetate (without acetic acid and alcohol). I think this drawback is solved in the process of hydrolysis when heated in the reaction mixture.
 

William D.

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In 10L flask it is better not to synthesize more than 80g p2np. For 2L flask are similar - it is better not to synthesize more than 15g and in the presence of experience. With experience, you can better control the reaction, but the amount of the above will be a great risk.
 

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 D.

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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.
 

nofuckups

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or just warming up the entire solution a bit before pouring into the aluminium amalgam?
 

timeandtime

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8:51 - what's the shelf life of the clear oil after it's been separated?
 

Chemdogkm

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most medication has shelf life 1 year,not that it doesnt work after just that it is recomended to use it before
 

New Student

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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 D.

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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.
 

New Student

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Thank you< so I probably don't need a fume hood for this
 

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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