Amfetamīna sintēze no P2NP, izmantojot Al/Hg (video)

[HIGGS BOSSON]

Video amfetamīnasintēzē tiek izmantoti reaģenti:

• 10 g 1-fenil-2-nitropropēna (P2NP);
• 100 ml izopropilspirta (IPA);
• 50 ml ledus etiķskābes (AcOH);
• 50 g nātrija hidroksīda (NaOH);
• 12 g alumīnija (sagrieztas sadzīves folijas veidā);
• 0,1 g dzīvsudraba (II) nitrāta (Hg(NO3)2);
• 2 ml sērskābes (H2SO4);
• 50 ml acetona;
• Destilēts ūdens;

Iekārtas un stikla trauki:

• Kolba ar plakanu dibenu, 2 l;
• Retorta statīvs un skava aparāta nostiprināšanai (pēc izvēles);
• Atpakaļplūsmas kondensators;
• piltuve;
• sieta filtrs (der virtuves filtrs);
• Šļirce vai Pastēra pipete;
• pH indikatora papīriņi;
• spaiņi (600 ml x2, 2 L, 1 L, 100 ml x2);
• Vakuuma avots;
• Laboratorijas svari (piemēroti 0,1-200 g);
• Mērcilindri 1000 ml un 100 ml;
• Aukstā ūdens vanna;
• Stikla stienis un lāpstiņa;
• 1 L dalāmā piltuve (pēc izvēles);
• laboratorijas termometrs;
• Bihnera kolba un piltuve;
• filtrpapīrs;

Amfetamīna sintēzes video apraksts.

Pirms sintēzes sākuma sagatavo 10 g 1-fenil-2-nitropropēna šķīdumu 100 ml izopropilspirta un 50 ml etiķskābes. Alumīnija amalgamas pagatavošanai arpapīra smalcinātāju sagriež sīkos gabaliņos arī alumīnija foliju 12 g . To var sagriezt ar šķērēm vai pārgriezt ar rokām (cimdos).

0:04-0:40 - Preparāta ūdens sārma šķīdums. Šis šķīdums tika pagatavots iepriekš, lai šķīdumam būtu istabas temperatūra līdz galvenajam reakcijas maisījuma sārmošanas laikam šajā video. Sārmošanu veic ar spontānu sildīšanu. Ja izmanto svaigu karstu sārmu šķīdumu, tad temperatūra paaugstināsies un būs nepieciešama reakcijas masas piespiedu dzesēšana.

0:46-2:36 - Amalgama ar dzīvsudraba nitrātu. Amalgamētais alumīnijs reducē 1-fenil-2-nitropropēnu līdz amfetamīnam. Amalgamēšanas reakcijas laikā izdalās neliels gāzes daudzums, veidojas pelēkas nogulsnes. Ir svarīgi nepalaist garām brīdi, kad alumīnija amalgama ir gatava. Šo brīdi var noteikt pēc pelēko nogulšņu veidošanās un pastiprinātas gāzes izdalīšanās. Tas notiek 10 līdz 15 minūšu laikā no reakcijas sākuma.

Ūdens tiek izlaists bez marles noņemšanas, amalgamētais alumīnijs tiek izskalots ar divām porcijām auksta destilēta ūdens. Jāpievērš uzmanība gāzes burbuļu izdalīšanai. Novēro, ka "pareizā" amalgamā burbuļi ir mazāki un šķidruma krāsa ir tumšāka. Ja reakcija ir strauja, burbuļi ir lieli un krāsa ir gaiša, amalgama ir "nepareiza". Tas gandrīz noteikti ir saistīts ar dzīvsudraba sāls trūkumu. Ņemiet vērā, ka dzīvsudraba sāļi ir indīgi.

2:37-4:28 - Vissvarīgākā procesa daļa ir 1-fenil-2-nitropropēna reducēšana ar alumīnija amalgamu. Reakcija ir eksotermiska, un tā notiek, izdalot daudz siltuma. Procedūras laikā rūpīgi jākontrolē temperatūra. Reakcijas kolbu pārkaršanas gadījumā atdzesē ledus vannā. Kolbā drīkst pievienot aukstu ūdeni. Dažreiz reakcija netiek uzsākta, reakcijas masa kārtīgi jāsasilda un reakcija jāuzsāk (ar pareizi sagatavotu amalgamu). Reakcijas laikā izdalās verdoša spirta un etiķskābes smarža. Tvaiku uztveršanai izmanto Allihn atgaitas kondensatoru. Allihn pretplūsmas kondensatora efektivitāti var palielināt, ja tam pieslēdz tekošu aukstu ūdeni.

5:04 - Reakcijas kolbu var izskalot ar nelielu daudzumu spirta, un ar to var izskalot arī nereaģējušo alumīniju, lai savāktu atlikumus un palielinātu iznākumu.

5:13 - Nereaģējušajam alumīnijam jābūt maz. Pēc atlikumiem var noteikt reaģējušā 1-fenil-2-nitropropēna daudzumu.

5:16-6:13 - Sārmojums. Reakciju veic ar siltuma izdalīšanu. Nereaģējušā alumīnija atliekas papildus reaģē ar sārmu un maisījumu uzkarsē, kā arī rada blakusproduktus.
30 minūšu laikā pēc sārmošanas notiek atdalīšanās redzamos slāņos. Augšējā slāņa pH jābūt 11-12.

6:18-7:23 - Dekantēšana. Savāc virsējo slāni ar amfetamīna bāzi spirtā. To var izžāvēt ar nelielu daudzumu bezūdens magnija sulfāta. Šlakvielas var ekstrahēt ar nepolāru šķīdinātāju (ēteri, benzolu, toluolu), tad šķīdinātāju iztvaicē.

7:24-8:50 - Sērskābes šķīduma sagatavošana acetonā. Šis šķīdums ir nepieciešams vienmērīgākai paskābināšanai. Ja izmanto koncentrētu sērskābi, notiek vietēja produkta pārskābošanās. Tādējādi samazinās iznākums.

8:51-10: 53 - Produkta paskābināšana un amfetamīna sulfāta iegūšana. Augšējam dzeltenajam slānim, kas tika savākts iepriekšējā posmā, pilienveidā pievieno sagatavotu sērskābes šķīdumu. Ar katru pilienu skābes šķīduma veidojas sāls pārslas. Šis posms ir ļoti svarīgs, rūpīgi jākontrolē pH, lai izvairītos no pārskābes. Skābināšanu turpina līdz pH 5,5 - 6. Pārskābinātam produktam ir sārta krāsa. Pilnīgas pārskābes gadījumā produkts bojājas.

10:55-11:38 - Amfetamīna sulfāta filtrēšana no šķīdinātājiem Bihnera piltuvē vakuumā. Šajā posmā produktu var papildus noskalot ar aukstu acetonu, izlejot to caur Buknera piltuvi kopā ar amfetamīna sulfāta kūku.

11:41-12:28 - Filtrēšana, izmantojot improvizētus instrumentus. Par filtru var izmantot jebkuru biezu audumu. Iegūto produktu vairākas stundas žāvē siltā un sausā vietā, lai atdalītu šķīdinātāju atliekas. Ieteicams to uzglabāt vakuuma iepakojumā.

Ieguvums ir 60-70 %.

 

[timeandtime]

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

 

[G.Patton]

Es varu jums palīdzēt ar sintēzi, jūs varat uzdot man privātās ziņās jebkuru jautājumu par.

 

[Barter]

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.]

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

 

[Eddybeaumont]

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]

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

 

[golab071]

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]

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

 

[William D.]

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]

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]

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

Start with smaller amount at first.

 

[Barter]

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]

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

 

[William D.]

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.]

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]

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]

yes, exactly.

 

[William D.]

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]

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

 

[timeandtime]

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

 

[Chemdogkm]

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

 

[timeandtime]

Thank you, helps a lot.

 

[New Student]

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.]

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]

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

 

[Chemdogkm]

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]

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

 

[golab071]

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]

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

 

[golab071]

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]

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]

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]

>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.