Amfetamino sintezė iš P2NP per Al/Hg (vaizdo įrašas)

[HIGGS BOSSON]

Vaizdo įraše amfetaminosintezė naudojami reagentai:

• 10 g 1-fenil-2-nitropropeno (P2NP);
• 100 ml izopropilo alkoholio (IPA);
• 50 ml ledinės acto rūgšties (AcOH);
• 50 g natrio hidroksido (NaOH);
• 12 g aliuminio (pjaustytos buitinės folijos pavidalu);
• 0,1 g gyvsidabrio (II) nitrato (Hg(NO3)2);
• 2 ml sieros rūgšties (H2SO4);
• 50 ml acetono;
• Distiliuotas vanduo;

Įranga ir stikliniai indai:

• 2 l plokščiadugnė kolba;
• Retorto stovas ir spaustukas aparatui pritvirtinti (neprivaloma);
• grįžtamasis kondensatorius;
• Piltuvėlis;
• Sietinis filtras (tinka virtuvinis);
• Švirkštas arba Pastero pipetė;
• pH indikatoriaus popierėliai;
• stiklinės (600 ml x2, 2 l, 1 l, 100 ml x2);
• Vakuumo šaltinis;
• Laboratorinės svarstyklės (tinka 0,1-200 g);
• 1000 mL ir 100 mL matavimo cilindrai;
• Šalto vandens vonia;
• Stiklinė lazdelė ir mentelė;
• 1 l atskiriamasis piltuvas (neprivalomas);
• Laboratorinis termometras;
• Buchnerio kolba ir piltuvas;
• Filtravimo popierius;

Amfetamino sintezės vaizdo įrašo aprašymas.

Prieš pradedant sintezę paruošiamas 10 g 1-fenil-2-nitropropeno tirpalas 100 ml izopropilo alkoholio ir 50 ml acto rūgšties. Be to, aliuminio amalgamai paruošti 12 g aliuminio folijos popieriaus smulkintuvu supjaustoma mažais gabalėliais . Ją galima kirpti žirklėmis arba plėšyti rankomis (mūvint pirštines).

0:04-0:40 - preparato vandeninis šarmo tirpalas. Šis tirpalas buvo pagamintas iš anksto, kad iki pagrindinio reakcijos mišinio šarminimo laiko šiame vaizdo įraše tirpalas turėtų kambario temperatūrą. Šarminimas atliekamas savaiminiu kaitinimu. Jei naudojamas šviežias karštas šarminis šarminis tirpalas, temperatūra pakyla aukščiau ir reikės priverstinio reakcijos masės aušinimo.

0:46-2:36 - Amalgama su gyvsidabrio nitratu. Amalgamuotas aliuminis redukuoja 1-fenil-2-nitropropeną iki amfetamino. Amalgamacijos reakcijos metu išsiskiria nedidelis kiekis dujų, susidaro pilkos nuosėdos. Svarbu nepraleisti momento, kai aliuminio amalgama yra paruošta. Šį momentą galima nustatyti pagal pilkų nuosėdų susidarymą ir padidėjusį dujų išsiskyrimą. Tai įvyksta per 10-15 minučių nuo reakcijos pradžios.

Vanduo išleidžiamas nenuėmus marlės, amalgamuotas aliuminis nuplaunamas dviem porcijomis šalto distiliuoto vandens. Verta atkreipti dėmesį į dujų burbuliukų išsiskyrimą. Pastebima, kad "teisingoje" amalgamoje burbuliukai yra mažesni, o skysčio spalva tamsesnė. Jei reakcija yra audringa, burbuliukai dideli, o spalva šviesi, amalgama yra "neteisinga". Tai beveik neabejotinai susiję su gyvsidabrio druskos trūkumu. Atkreipkite dėmesį, kad gyvsidabrio druskos yra nuodingos.

2:37-4:28 - Svarbiausia proceso dalis yra 1-fenil-2-nitropropeno redukcija aliuminio amalgama. Reakcija yra egzoterminė ir vyksta gausiai išsiskiriant šilumai. Procedūros metu būtina atidžiai kontroliuoti temperatūrą. Reakcijos kolba perkaitimo atveju aušinama ledo vonelėje. Į kolbą leidžiama įpilti šalto vandens. Kartais reakcija neprasideda, būtina gerai pašildyti reakcijos masę ir reakcija pradedama (su tinkamai paruošta amalgama). Reakcijos metu išsiskiria verdančio alkoholio ir acto rūgšties kvapai. Garams surinkti naudojamas Alihno grįžtamasis kondensatorius. Allihn grįžtamojo kondensatoriaus efektyvumą galima padidinti prie jo prijungus tekantį šaltą vandenį.

5:04 - Reakcijos kolbą galima išplauti nedideliu kiekiu alkoholio, o nesureagavusį aliuminį taip pat galima išplauti juo, kad būtų surinktos liekanos ir padidinta išeiga.

5:13 - Nesureagavusio aliuminio turėtų likti nedaug. Pagal likučius galima nustatyti sureagavusio 1-fenil-2-nitropropeno kiekį.

5:16-6:13 - Šarminimas. Reakcija vykdoma su šilumos išleidimu. Nesureagavusio aliuminio likučiai papildomai reaguoja su šarmu ir įkaitina mišinį, taip pat susidaro šalutiniai produktai.
Po šarminimo per 30 minučių įvyksta atskyrimas į matomus sluoksnius. Viršutinio sluoksnio pH turi būti 11-12.

6:18-7:23 - Dekantavimas. Surinkite viršutinį sluoksnį su amfetamino baze alkoholyje. Jį galima išdžiovinti nedideliu kiekiu bevandenio magnio sulfato. Šlaką galima ekstrahuoti nepoliniu tirpikliu (eteriu, benzenu, toluenu), tada išgarinti tirpiklį.

7:24-8:50 - Sieros rūgšties tirpalo acetone paruošimas. Šis tirpalas reikalingas sklandesniam parūgštinimui. Jei naudojama koncentruota sieros rūgštis, įvyksta vietinis produkto perrūgštinimas. Todėl sumažėja išeiga.

8:51-10:53 - Produkto parūgštinimas ir amfetamino sulfato gavimas. Į viršutinį geltoną sluoksnį, kuris buvo surinktas ankstesniame etape, lašiniu būdu įlašinamas paruoštas sieros rūgšties tirpalas. Su kiekvienu rūgšties tirpalo lašu susidaro druskos dribsniai. Šis etapas yra labai svarbus, būtina atidžiai kontroliuoti pH, kad būtų išvengta per didelio rūgštingumo. Rūgštinimas tęsiamas tol, kol pasiekiamas pH 5,5-6. Perrūgštintas produktas yra rausvos spalvos. Visiškai perrūgštinus produktas bus sugadintas.

10:55-11:38 - amfetamino sulfato filtravimas iš tirpiklių Buchnerio piltuve vakuume. Šiame etape produktą galima papildomai nuplauti šaltu acetonu, perpilant jį per Buchnerio piltuvą su amfetamino sulfato pyragu.

11:41-12:28 - Filtravimas naudojant improvizuotus įrankius. Kaip filtrą galima naudoti bet kokį storą audinį. Gautas produktas kelias valandas džiovinamas šiltoje ir sausoje vietoje, kad būtų pašalinti tirpiklių likučiai. Rekomenduojama jį laikyti vakuuminėje pakuotėje.

Išeiga 60-70 %.

 

[timeandtime]

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

 

[G.Patton]

Galiu jums padėti su sinteze, galite užduoti man privačiomis žinutėmis bet kokį klausimą apie.

 

[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.