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Síntesis de anfetamina a partir de P2NP mediante Al/Hg (vídeo)

HIGGS BOSSON

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En el vídeo de síntesis de la anfetamina se utilizan reactivos:
  • 10 g de1-fenil-2-nitropropeno (P2NP);
  • 100 ml de alcohol isopropílico (IPA);
  • 50 ml de ácido acético glacial (AcOH);
  • 50 g Hidróxido de sodio (NaOH);
  • 12 g Aluminio (en forma de papel de aluminio doméstico cortado);
  • 0,1 g de nitrato de mercurio (II) (Hg(NO3)2);
  • 2 ml Ácido sulfúrico (H2SO4);
  • 50 ml de acetona;
  • Agua destilada;
Equipo y cristalería:
  • Matraz de fondo plano de 2 L;
  • Soporte de retorta y abrazadera para fijar el aparato (opcional);
  • Condensador de reflujo;
  • Embudo;
  • Filtro de tamiz (el de cocina está bien);
  • Jeringa o pipeta Pasteur;
  • Papel indicadordel pH;
  • Vasos de precipitados (600 mL x2, 2 L, 1 L, 100 mL x2);
  • Fuente de vacío;
  • Balanza de laboratorio (0,1-200 g es adecuada);
  • Probetas graduadas de 1000 mL y 100 mL;
  • Baño de agua fría;
  • Varilla de vidrio y espátula;
  • Embudo de decantación de 1 L (opcional);
  • Termómetro de laboratorio;
  • Matraz Buchner y embudo;
  • Papel de filtro;

7sbroyikpe

Descripción del vídeo de síntesis de anfetamina.
Antes de comenzar la síntesis se prepara una solución de 1-fenil-2-nitropropeno 10 g en 100 ml de alcohol isopropílico y 50 ml de ácido acético. Además, se corta en trozos pequeños una lámina de aluminio de 12 g con una trituradora de papel para preparar una amalgama de aluminio. Se puede cortar con tijeras o rasgar con las manos (con guantes).

0:04-0:40 - Una solución alcalina acuosa de preparación. Esta solución se hizo de antemano para que la solución tiene temperatura ambiente por la mezcla de reacción principal tiempo de alcalinización en este video. La alcalinización se lleva a cabo con un calentamiento espontáneo. Si se utiliza una solución alcalina aq caliente fresca, entonces la temperatura se eleva más y será necesario un enfriamiento forzado de la masa de reacción.

0:46-2:36 - Amalgama con nitrato de mercurio.
El aluminio amalgamado reducirá el 1-fenil-2-nitropropeno a anfetamina. Durante la reacción de amalgamación se desprende una pequeña cantidad de gas y se forma un precipitado gris. Es importante no perderse el momento en que la amalgama de aluminio está lista. Este momento puede determinarse por la formación de un precipitado gris y por un aumento de la evolución del gas. Ocurre en 10-15 minutos desde el inicio de la reacción.

Se escurre el agua sin retirar una gasa, se lava el aluminio amalgamado con dos porciones de agua destilada fría. Vale la pena prestar atención al desprendimiento de burbujas de gas. Se nota que las burbujas son más pequeñas y el color del líquido es más oscuro en una amalgama "correcta". Si la reacción es violenta, las burbujas son grandes y el color es claro, la amalgama es "incorrecta". Esto se debe casi con toda seguridad a la falta de sales de mercurio. Tenga en cuenta que las sales de mercurio son venenosas.

2:37-4:28 - La parte más importante del proceso es la reducción del 1-fenil-2-nitropropeno por la amalgama de aluminio. La reacción es exotérmica y se lleva a cabo con abundante desprendimiento de calor. Es necesario controlar cuidadosamente la temperatura durante el procedimiento. El matraz de reacción se enfría en un baño de hielo en caso de sobrecalentamiento. Se permite añadir agua fría al matraz. A veces no se inicia la reacción, es necesario calentar bien la masa de reacción y se inicia la reacción (con una amalgama debidamente preparada). Durante la reacción se desprenden olores de alcohol hirviendo y ácido acético.
Elcondensador de reflujo Allihn se utiliza para capturar los vapores. La eficacia del condensador de reflujo Allihn puede aumentarse con agua fría corriente, que puede conectarse a él.

5:04 - El matraz de reacción puede enjuagarse con una pequeña cantidad de alcohol y el aluminio sin reaccionar puede enjuagarse también con él para recoger los residuos y aumentar el rendimiento.

5:13 - Debería quedar poco aluminio sin reaccionar. Se puede determinar la cantidad de 1-fenil-2-nitropropeno reaccionado por los residuos.

5:16-6: 13 - Alcalinización. La reacción se lleva a cabo con un desprendimiento de calor. Los restos de aluminio no eliminados reaccionarán adicionalmente con el álcali y calentarán la mezcla, además de crear subproductos.
La separación en capas visibles se produce en los 30 minutos siguientes a la alcalinización. El
pH de la capa superior debe ser de 11-12.

6:18-7:23 -
Decantación. Recoger la capa superior con base de anfetamina en alcohol. Se puede secar con una pequeña cantidad de sulfato de magnesio anhidro. La escoria se puede extraer con un disolvente no polar (éter, benceno, tolueno), luego se evapora un disolvente.

7:24-8:50 - Preparación de la solución de ácido sulfúrico en acetona. Esta solución es necesaria para una acidificación más suave. Si se utiliza ácido sulfúrico concentrado, se produce una sobreacidificación local del producto. Por lo tanto, el rendimiento disminuye.

8:51-10:53 - Acidificación del producto y obtención del sulfato de anfetamina. A la capa amarilla superior, que se recogió en la etapa anterior, se añade gota a gota una solución preparada de ácido sulfúrico. Con cada gota de solución ácida se forman escamas de sal. Esta etapa es muy importante, es necesario controlar cuidadosamente el pH para evitar una acidificación excesiva. La acidificación se continúa hasta
unpH de 5,5-6. El producto sobreacidificado tiene un color rosáceo. El producto se estropeará en caso de sobreacidificación total.

10:55-11:38 -
Filtración del sulfato de anfetamina de los disolventes en un embudo Buchner al vacío. El producto puede aclararse adicionalmente con acetona fría en esta fase, vertiéndolo a través de un embudo Buchner con la torta de sulfato de anfetamina.

11:41 -12:28 - Filtración utilizando herramientas improvisadas. Se puede utilizar cualquier tela gruesa como filtro. El producto resultante se seca en un lugar cálido y seco durante varias horas para eliminar los disolventes residuales.
Se recomienda almacenarlo en un envase al vacío.

El rendimiento es del 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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Puedo ayudarte con la síntesis, puedes preguntarme en mensajes privados cualquier duda sobre.
 

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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