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Syntéza amfetamínu z P2NP prostredníctvom Al/Hg (video)

HIGGS BOSSON

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Vo videosyntéze amfetamínu sa používajú činidlá:
  • 10 g 1-fenyl-2-nitropropénu (P2NP);
  • 100 ml izopropylalkoholu (IPA);
  • 50 ml ľadovej kyseliny octovej (AcOH);
  • 50 g hydroxidu sodného (NaOH);
  • 12 g hliníka (vo forme plátkov fólie pre domácnosť);
  • 0,1 g dusičnanu ortuťnatého (II) (Hg(NO3)2);
  • 2 ml kyseliny sírovej (H2SO4);
  • 50 ml acetónu;
  • Destilovaná voda;
Vybavenie a sklenené nádoby:
  • Sklenená banka s plochým dnom 2 l;
  • Retortový stojan a svorka na upevnenie prístroja (voliteľné);
  • spätný chladič;
  • lievik;
  • Sitový filter (kuchynský filter je vhodný);
  • Striekačka alebo Pasteurova pipeta;
  • papiere s indikátorompH;
  • kadičky (600 ml x2, 2 l, 1 l, 100 ml x2);
  • Zdroj vákua;
  • laboratórne váhy (vhodné 0,1 - 200 g);
  • Odmerné valce s objemom 1000 ml a 100 ml;
  • Studený vodný kúpeľ;
  • Sklenená tyčinka a špachtľa;
  • Oddeľovací lievik 1 l (voliteľný);
  • laboratórny teplomer;
  • Buchnerova banka a lievik;
  • filtračný papier;

7sbroyikpe

Opis videa syntézy amfetamínu.
Pred začiatkom syntézy sa pripraví roztok 1-fenyl-2-nitropropénu 10 g v 100 ml izopropylalkoholu a 50 ml kyseliny octovej. Taktiež sa skartovačkou papiera nastrúha hliníková fólia 12 g na malé kúsky na prípravu hliníkového amalgámu. Môže sa strihať nožnicami alebo trhať rukami (v rukaviciach).

0:04-0:40 - Vodný roztok alkalického prípravku. Tento roztok bol pripravený vopred, aby mal roztok izbovú teplotu do času alkalizácie hlavnej reakčnej zmesi v tomto videu. Alkalizácia sa vykonáva samovoľným zahrievaním. Ak sa použije čerstvý horúci alkalický roztok, teplota stúpne vyššie a bude potrebné nútené ochladenie reakčnej hmoty.

0:46 - 2:36 - Amalgám s dusičnanom ortuťnatým. Amalgamovaný hliník zredukuje
1-fenyl-2-nitropropén na amfetamín. Počas amalgamačnej reakcie sa uvoľňuje malé množstvo plynu, vzniká sivá zrazenina. Je dôležité nepremeškať okamih, keď je hliníkový amalgám hotový. Tento okamih možno určiť podľa tvorby sivej zrazeniny a zvýšeného vývinu plynu. Stane sa to za 10 až 15 minút od začiatku reakcie.

Voda sa vypustí bez odstránenia gázy, amalgamovaný hliník sa premyje dvoma dávkami studenej destilovanej vody. Je potrebné venovať pozornosť uvoľňovaniu plynových bublín. Všimnite si, že bublinky sú menšie a farba kvapaliny je tmavšia v "správnom" amalgáme. Ak je reakcia prudká, bubliny sú veľké a farba je svetlá, amalgám je "nesprávny". Je to takmer určite spôsobené nedostatkom ortuťovej soli. Upozorňujeme, že ortuťové soli sú jedovaté.

2:37-4:28 - Najdôležitejšoučasťou procesu je redukcia 1-fenyl-2-nitropropénu hliníkovým amalgámom. Reakcia je exotermická a prebieha za výdatného uvoľňovania tepla. Počas postupu je potrebné starostlivo kontrolovať teplotu. Reakčná banka sa v prípade prehriatia chladí v ľadovom kúpeli. Do banky sa môže pridať studená voda. Niekedy sa reakcia nespustí, je potrebné reakčnú hmotu dôkladne zohriať a reakcia sa spustí (so správne pripraveným amalgámom). Počas reakcie sa uvoľňuje zápach vriaceho alkoholu a kyseliny octovej.
Na zachytenie pár sa používa Allihn refluxný kondenzátor. Účinnosť Allihn refluxného kondenzátora možno zvýšiť tečúcou studenou vodou, ktorá sa k nemu môže pripojiť.

5:04 - Reakčnú banku možno vypláchnuť malým množstvom alkoholu a nezreagovaný hliník sa ním môže tiež vypláchnuť, aby sa zachytili zvyšky a zvýšil výťažok.

5:13 - Nezreagovaného hliníka by malo zostať málo. Množstvo zreagovaného 1-fenyl-2-nitropropénu môžete určiť podľa zvyškov.

5:16-6:13 - Alkalizácia. Reakcia prebieha s uvoľňovaním tepla. Zvyšky nezreagovaného hliníka dodatočne reagujú so zásadou a zahrievajú zmes, ako aj vytvárajú vedľajšie produkty.
K rozdeleniu na viditeľné vrstvy dochádza do 30 minút po alkalinizácii.
pH vrchnej vrstvy by malo byť 11 - 12.

6:18 - 7:23 -
Dekantácia. Zoberte vrchnú vrstvu s amfetamínovou bázou v alkohole. Môže sa vysušiť malým množstvom bezvodého síranu horečnatého. Trosku možno extrahovať nepolárnym rozpúšťadlom (éter, benzén, toluén), potom sa rozpúšťadlo odparí.

7:24 - 8:50 - Príprava roztoku kyseliny sírovej v acetóne. Tento roztok je potrebný na hladšie okyslenie. Ak sa použije koncentrovaná kyselina sírová, dôjde k lokálnemu prekysleniu produktu. Preto výťažok klesá.

8:51-10: 53 - Okyslenie produktu a získanie amfetamínsulfátu. K hornej žltej vrstve, ktorá bola zachytená v predchádzajúcej fáze, sa po kvapkách pridá pripravený roztok kyseliny sírovej. S každou kvapkou roztoku kyseliny sa vytvoria vločky soli. Táto fáza je veľmi dôležitá, je potrebné starostlivo kontrolovať pH, aby sa zabránilo nadmernému okysleniu. V okysľovaní sa pokračuje až do
pH 5,5 - 6. Prekyslený produkt má ružovkastú farbu. V prípade úplného prekyslenia sa produkt pokazí.

10:55 - 11:38 -
Filtrácia amfetamín sulfátu z rozpúšťadiel v Buchnerovom lieviku vo vákuu. Produkt sa môže v tejto fáze dodatočne opláchnuť studeným acetónom tak, že sa preleje cez Buchnerov lievik s koláčom amfetamín sulfátu.

11:41-12:28 - Filtrácia pomocou improvizovaných nástrojov. Ako filter sa môže použiť akákoľvek hrubá tkanina. Výsledný produkt sa niekoľko hodín suší na teplom a suchom mieste, aby sa odstránili zvyšky rozpúšťadiel. Odporúča sa skladovať ho vo vákuovom obale.

Výťažok je 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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Môžem vám pomôcť so syntézou, v súkromných správach mi môžete položiť akúkoľvek otázku týkajúcu sa.
 

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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