Amfetaminsyntes från P2NP via Al/Hg (video)

HIGGS BOSSON

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I videon om syntes avamfetamin används reagenser:
  • 10 g 1-fenyl-2-nitropropen ( P2NP);
  • 100 ml isopropylalkohol (IPA);
  • 50 ml Glacial ättiksyra (AcOH);
  • 50 g natriumhydroxid (NaOH)
  • 12 g aluminium (i form av skivad hushållsfolie)
  • 0,1 g kvicksilver(II)nitrat (Hg(NO3)2)
  • 2 ml svavelsyra (H2SO4)
  • 50 ml aceton;
  • Destillerat vatten;
Utrustning och glasvaror:

7sbroyikpe

Beskrivning av video om amfetaminsyntes.
En lösning av 1-fenyl-2-nitropropen 10 g i 100 ml isopropylalkohol och 50 ml ättiksyra bereds innan syntesen startar. Dessutom skärs en aluminiumfolie 12 g i små bitar med en pappersförstörare för en aluminiumamalgamberedning. Den kan klippas med sax eller rivas med händerna (i handskar).

0:04-0:40 - En vattenhaltig alkalilösning för beredning. Denna lösning gjordes i förväg så att lösningen har rumstemperatur vid huvudreaktionsblandningens alkaliseringstid i den här videon. Alkaliniseringen utförs med en spontan uppvärmning. Om en ny varm aq alkalilösning används, stiger temperaturen högre och en tvingad kylning av reaktionsmassan kommer att krävas.

0:46-2:36 - Amalgam med kvicksilvernitrat. Amalgamerat aluminium reducerar
1-fenyl-2-nitropropen till amfetamin. En liten mängd gas utvecklas under amalgamreaktionen, en grå fällning bildas. Det är viktigt att inte missa ögonblicket när aluminiumamalgamet är färdigt. Detta ögonblick kan bestämmas av en grå fällningsbildning och av en ökad gasutveckling. Det sker inom 10-15 minuter från reaktionsstart.

Vattnet dräneras utan att en gasbinda avlägsnas, det amalgamerade aluminiumet tvättas med två portioner kallt destillerat vatten. Det är värt att vara uppmärksam på att gasbubblorna släpper. Det märks att bubblorna är mindre och vätskans färg är mörkare i ett "korrekt" amalgam. Om reaktionen är våldsam, bubblorna är stora och färgen är ljus, är amalgamet "felaktigt". Detta beror nästan säkert på brist på kvicksilversalt. Observera att kvicksilversalter är giftiga.

2:37-4:28 - Den viktigaste delen av processen är reduktion av 1-fenyl-2-nitropropen med aluminiumamalgam. Reaktionen är exoterm och utförs med en riklig värmeavgivning. Det är nödvändigt att noggrant kontrollera temperaturen under proceduren. Reaktionsflaskan kyls i ett isbad i händelse av överhettning. Det är tillåtet att tillsätta kallt vatten i kolven. Ibland startar inte reaktionen, då är det nödvändigt att värma reaktionsmassan ordentligt och reaktionen startar (med ett korrekt förberett amalgam). Lukt av kokande alkohol och ättiksyra frigörs under reaktionen.
Allihn återflödeskondensor används för att fånga upp ångor. Effektiviteten hos Allihns återflödeskondensor kan ökas med rinnande kallt vatten, som kan anslutas till den.

5:04 - Reaktionskolven kan sköljas med en liten mängd alkohol och oreducerat aluminium kan också sköljas med det för att samla upp rester och öka utbytet.

5:13 - Det bör finnas lite oreducerat aluminium kvar. Du kan bestämma mängden reagerad 1-fenyl-2-nitropropen med hjälp av restprodukterna.

5:16-6:13 - Alkalinisering. Reaktionen utförs med en värmefrigöring. Resterna av oredigerat aluminium kommer dessutom att reagera med alkali och värma blandningen samt skapa biprodukter.
En separation i synliga skikt sker inom 30 minuter efter alkalinisering.
pH-värdet i det översta skiktet ska vara 11-12.

6:18-7:23 -
Dekantera. Samla upp det översta skiktet med amfetaminbas i alkohol. Det kan torkas med en liten mängd vattenfritt magnesiumsulfat. Slaggen kan extraheras med ett icke-polärt lösningsmedel (eter, bensen, toluen), sedan indunstas ett lösningsmedel.

7:24-8:50 - Beredning av svavelsyralösningen i aceton. Denna lösning är nödvändig för en smidigare surgöring. Om koncentrerad svavelsyra används sker en lokal översyrning av produkten. Därför sjunker utbytet.

8:51-10:53 - Produktens surgörning och erhållande av amfetaminsulfat. Till det övre gula skiktet, som samlades upp i föregående steg, tillsätts droppvis en beredd lösning av svavelsyra. Saltflingor bildas med varje droppe syralösning. Detta steg är mycket viktigt, det är nödvändigt att noggrant kontrollera pH för att undvika översyra. Försurningen fortsätter
tillpH 5,5-6. Den översyrade produkten har rosa färg . Produkten kommer att förstöras vid en total översyrning.

10:55-11:38 -
Amfetaminsulfatfiltrering från lösningsmedel i en Buchner-tratt under vakuum. Produkten kan dessutom sköljas med kall aceton i detta skede genom att hälla den genom Buchner-tratten med amfetaminsulfatkakan.

11:41-12:28 - Filtrering med hjälp av improviserade verktyg. Alla tjocka tyger kan användas som filter. Den resulterande produkten torkas på en varm och torr plats i flera timmar för att avlägsna resterande lösningsmedel.
Vi rekommenderar att den förvaras i en vakuumförpackning.

Utbytet är 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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Jag kan hjälpa dig med syntes, du kan fråga mig i privata meddelanden någon fråga om.
 

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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