Amfetamiini süntees P2NP-st Al/Hg abil (video)

[HIGGS BOSSON]

Videosünteesi puhul kasutatakseamfetamiini reagente:

• 10 g 1-fenüül-2-nitropeeni (P2NP);
• 100 ml isopropüülalkoholi (IPA);
• 50 ml jäääädikhapet (AcOH);
• 50 g naatriumhüdroksiidi (NaOH);
• 12 g alumiiniumi (viilutatud majapidamisfooliumi kujul);
• 0,1 g elavhõbe(II)nitraat (Hg(NO3)2);
• 2 ml väävelhapet (H2SO4);
• 50 ml atsetooni;
• Destilleeritud vesi;

Seadmed ja klaastooted:

• 2 l lamedapõhjaline kolb;
• Retordialus ja klamber seadme kinnitamiseks (valikuline);
• tagasivoolukondensaator;
• Trummel;
• Sõelfilter (köögis kasutamiseks sobib);
• Süstel või pastör-pipett;
• pH-indikaatorpaberid;
• keeduklaasid (600 mL x2, 2 L, 1 L, 100 mL x2);
• Vaakumiallikas;
• laborikaal (sobib 0,1-200 g);
• Mõõtesilindrid 1000 ml ja 100 ml;
• Külmaveevann;
• Klaasvarda ja spaatel;
• eraldussahtel 1 L (valikuline);
• Laboratoorne termomeeter;
• Buchneri kolb ja lehter;
• Filtripaber;

Amfetamiini sünteesi video kirjeldus.

Enne sünteesi algust valmistatakse 1-fenüül-2-nitropeeni 10 g lahus 100 ml isopropüülalkoholi ja 50 ml äädikhappe lahus. Samuti lõigatakse alumiiniumfoolium 12 g alumiiniumamalgaami valmistamiseks paberilõikuriga väikesteks tükkideks . Seda võib lõigata kääridega või rebida kätega (kinnastega).

0:04-0:40 - preparaadi vesialuselise leelise lahus. See lahus valmistati eelnevalt nii, et lahus on toatemperatuuril põhireaktsioonisegu leelestamise ajaks selles videos. Leelestamine toimub spontaanse kuumutamisega. Kui kasutatakse värsket kuuma aq leeliselahust, siis tõuseb temperatuur kõrgemale ja vajalik on reaktsioonimassi sundjahutamine.

0:46-2:36 - Amalgaam elavhõbedanitraadiga. Amalgaamitud alumiinium redutseerib 1-fenüül-2-nitropeeniamfetamiiniks. Amalgaamimisreaktsiooni käigus eraldub väike kogus gaasi, moodustub hall sade. Oluline on, et alumiiniumamalgaami valmimise hetk ei jääks vahele. Seda hetke saab kindlaks teha halli sette tekkimise ja suurenenud gaasievolutsiooni järgi. See juhtub 10-15 minuti jooksul alates reaktsiooni algusest.

Vesi lastakse ära ilma marli eemaldamata, amalgaamitud alumiinium pestakse kahe portsjoni külma destilleeritud veega. Tähelepanu tasub pöörata gaasimullide vabanemisele. On märgata, et mullid on väiksemad ja vedeliku värvus on tumedam "õiges" amalgaamis. Kui reaktsioon on äge, mullid on suured ja värvus on hele, on amalgaam "vale". See on peaaegu kindlasti tingitud elavhõbedasoola puudumisest. Pange tähele, et elavhõbedasoolad on mürgised.

2:37-4:28 - Protsessi kõige olulisem osa on 1-fenüül-2-nitropropeeni redutseerimine alumiiniumamalgaami abil. Reaktsioon on eksotermiline ja toimub rohke soojuse eraldumisega. Protseduuri käigus tuleb temperatuuri hoolikalt kontrollida. Ülekuumenemise korral jahutatakse reaktsioonikolbi jäävannis. Kolbi lubatakse lisada külma vett. Mõnikord ei käivitata reaktsiooni, tuleb reaktsioonimassi põhjalikult soojendada ja reaktsioon käivitada (korralikult ettevalmistatud amalgaamiga). Reaktsiooni ajal eraldub keeva alkoholi ja äädikhappe lõhn. Allihn tagasivoolukondensaatorit kasutatakse aurude püüdmiseks. Allihn reflukskondensaatori tõhusust saab suurendada külma vee jooksmisega, mille võib ühendada sellega.

5:04 - Reaktsioonikolbi võib loputada väikese koguse alkoholiga ja sellega võib loputada ka reageerimata alumiiniumi, et koguda jääke ja suurendada saagist.

5:13 - Reageerimata alumiiniumi peaks jääma vähe. Reageerinud 1-fenüül-2-nitropeeni kogust saab määrata jääkide järgi.

5:16-6:13 - Alkaliseerimine. Reaktsioon viiakse läbi soojuse vabastamisega. Redutseerimata alumiiniumi jäägid reageerivad täiendavalt leelisega ja kuumutavad segu ning tekitavad kõrvalsaadusi.
30 minuti jooksul pärast leelistamist toimub eraldumine nähtavateks kihtideks. Ülemise kihi pH peaks olema 11-12.

6:18-7:23 - Dekanteerimine. Koguda ülemine kiht koos amfetamiini alusega alkoholis. Seda võib kuivatada väikese koguse veevaba magneesiumsulfaadiga. Kihti võib ekstraheerida mittepolaarse lahustiga (eeter, benseen, tolueen), seejärel aurustatakse lahusti.

7:24-8:50 - Väävelhappe lahuse valmistamine atsetoonis. See lahus on vajalik sujuvamaks hapestamiseks. Kui kasutatakse kontsentreeritud väävelhapet, toimub toote kohalik ülehapestumine. Seetõttu väheneb saagis.

8:51-10:53 - Toote hapestamine ja amfetamiinsulfaadi saamine. Eelmises etapis kogutud ülemisele kollasele kihile lisatakse tilkhaaval ettevalmistatud väävelhappe lahust. Iga happelahuse tilgaga moodustuvad soola helbed. See etapp on väga oluline, pH-d tuleb hoolikalt kontrollida, et vältida ülehapestumist. Hapestamist jätkatakse, kuni pH on 5,5-6. Ülehapestatud toode on roosa värvi. Täieliku ülehapestamise korral toode rikneb.

10:55-11:38 - amfetamiinsulfaadi filtreerimine lahustitest Buchneri nõelas vaakumis. Selles etapis võib toodet täiendavalt loputada külma atsetooniga, valades selle koos amfetamiinsulfaadi koogiga läbi Buchneri lehtri.

11:41-12:28 - Filtreerimine improviseeritud vahenditega. Filtrina võib kasutada mis tahes paksu kangast. Saadud toode kuivatatakse kuivas ja soojas kohas mitu tundi, et eemaldada lahusti jäägid. Soovitatav on säilitada seda vaakumpakendis.

Saagis on 60-70%.

 

[timeandtime]

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

 

[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?

 

[William Dampier]

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.

 

[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 Dampier]

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 Dampier]

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.

 

[whyicantmakeit09]

Can I substitute DCM for Acetone in Amphetamine Synthesis?

Hey fellow chemists!

I'm currently working through an amphetamine synthesis protocol (thanks to Amine expert guidance) and I'm curious about substituting dichloromethane (DCM) for acetone. Specifically, I'm wondering if it's possible to use DCM as a replacement in the following steps:

• 
  
• Work-up: after extracting with DCM, could I use it again to wash the organic layer instead of acetone?

I understand that DCM is generally less polar than Acetone, so I'm worried about potential issues with solubility or contamination. Has anyone tried substituting DCM in this protocol before? Are there any specific concerns I should be aware of?

Thanks for sharing your experiences and expertise!

 

[Chemdogkm]

Yes u can use about any solvent for cleaning