Ühe poti amfetamiini süntees P2NP-st NaBH4/CuCl2-ga (1kg skaala)

[Montecristo]

Siin oli see, mida ma väiksemas mahus tegin;
1. Lahus IPA/H2O 2:1 ((IPA 800ml,H2O 400ml)(1200ml)) lisati 2000ml kolbi.
2. Lisati kohe NaBH4 (116 g) ja alustati segamist.
3. P2NP (67 g) lisati väikestes annustes, nii et segu temperatuur ei ületaks 60 *С.
4. CuCl2 (7 g) vees (13 ml) lisati aeglaselt tilguti, nii et segu temperatuur ei ületaks 80 *С.
5. Seejärel reostati reaktsiooni 80 °C juures 30 minutit välisküttega.
6. Lahus dekanteeriti ja filtreeriti reaktsioonijäätmetest ning pandi eraldussahtrisse.
7. Reaktsioonisegule lisati NaOH 25%-line vesilahus (533 ml) ja faasid eraldati.
8. Alumine kiht kurnatakse suurde keeduklaasi ja kogutakse ülemine orgaaniline kiht.
9. Seejärel pandi vesifaas eraldussahtrisse ja ekstraheeriti 500 ml IPAga.
10. IPA aurustati 3/4 ulatuses, pooleldi piimjas vababaas ja pooleldi IPA.
11.IPA ja freebase lahustati 130 ml atsetoonis.
12.ortofosforhapet tilguti pH-ni - 6 (pideva segamise juures).
13.segu pandi 12 tunniks sügavkülma.
14.Pärast kristalliseerumist suspensioon filtreeriti ja pesti kuiva külma atsetooniga, kuni atsetoon on puhas.
15.Pesemisest saadud atsetoon ja ipa/atsetooni segu pannakse tagasi sügavkülma edasiseks sadestamiseks.
16.Protsessi korratakse, kuni ei teki enam sadet, et saada 60-70% kvaliteetset amfetamiini, kuna segusse satub rohkem atsetooni, võib olla vaja tilgutada veel veidi hapet, et seda vähendada, kuid mitte liiga palju, kuna atsetoon on ph7.

Siin on foto mõnest kuivatatud pastakivist , ülejäänud on kuiv pulber, mida tuleb segada, kuna see on minu ja mu sõprade jaoks liiga tugev.
Ma võin retsepti uuendada ja teha kirjutama väikesemahulise kodukeemia jaoks, seal on palju võimalusi, kuidas see võiks olla parem.

 

[flyhigh]

see ei ole met , saate siit kirjutada, kuidas teha seda kristallmetalliks

 

[Kylemalone1297]

A different process. P2P or sudo. Just pick one. But these are safer imo

 

[G.Patton]

Tere. CuCl2 Toimib selles reaktsioonis katalüsaatorina. Kas vajate üksikasjalikumat selgitust?

 

[Kylemalone1297]

I would like to know the entire concept if u k know it. Like how much copper to reduce p2np exactly. Are we making an electron here in this synth? What is going on exactly ? I understand how to run through but not the actual chemical reaction that is happening.

 

[G.Patton]

What do you mean?
There is clearly said how much. 105g CuCl2 per 1kg P2NP.

NaBH4 donate hydrogen while this reaction to P2NP and nitrogen atom change its oxidation state from +3 to -3. Hence, it get 6 electrons.

 

[mithyl2]

ja millist % väävelhapet tuleks kasutada?

 

[Kylemalone1297]

Buy virgin sulfuric from as drain cleaner if u can’t find one with a high purity. I could only find like 20% online for some reason. The drain cleaner is actualy more pure. Like wtf

 

[G.Patton]

it's worth to use 96-98%, but you can use less concentrated as well.

 

[diogenes]

Tere,

Tegin just selle sünteesi ja saagis on 60%+ (osa atsetooni veel sügavkülmikus), mis ei ole halb, arvestades, et mingil hetkel reaktsioonimass lekkis välja (ülekuumenes ja hakkas paisuma). Ma jahutasin seda kiiresti ja siis hoidsin reflukskondensaatorit üleval ülejäänud reaktsiooni ajal (algses kirjelduses seda ei mainita). Pärast P2NP osa lisamist on soojuse suurenemine veidi hilinenud, mida tuleb arvestada, ma lisasin veel ühe osa liiga kiiresti. Külmavann on mugav. Lõpptoode on biotesti mõttes väga tõhus, ma teen happe-baasi ekstraheerimist, et näha, kas lõpptoode on ka muud kemikaalid. On kerge, selge lõhn, mida ma identifitseerin kui Cu lõhna lähedal ehk?, mis püsib vaatamata 5X atsetooniga pesemisele ja millel on väga valge, puhta väljanägemisega toode.

Ma mõtlesin, kas siin on keegi, kes võiks kirjutada välja täpse reaktsiooni, mis toimub selles sünteesis. CuCl2 roll ei ole mulle selge ja ka see, kuidas H aatomid liiguvad jne. Oleks väga kasulik, kui reaktsioon oleks natuke täpsemalt lahti seletatud. Vabandan, kui seda on juba mainitud, olen enamuse sellest teemast näinud, aga pole viimasel ajal jõudnud järele jõuda. Tänan teid

 

[mile123]

Hello!

What reflux condenser do you recommend, is Friedrichs really worth double the price compared to Graham?

Condensers

Laborxing.com, one stop online shop for lab glasses, lab equipment and chemicals.

www.laborxing.com

I read here that @OrgUnikum recommends Friedrichs.


I'm thinking about adding reflux condenser at 3. step

because of suggestion below

and possible h2 production safety reasons


Br,
Mile

 

[WinterDust]

Praegu teen 200 g P2nP partiisid.

Mul on üsna hea jahutusmeetod, nii et minu temperatuur ei ületa kunagi 47celsius.

Kogu 200g portsjoni lisamiseks kulub 1h.

Pärast P2nP lisamist võtab reaktsioon veidi aega, et esimene kord toimuks ja see hakkab vahutama, vahutamise ajal. Ärge lisage rohkem P2nP-d! Oodake, kuni vaht settib ja te näete 60% vahtu ja 40% vedelikku, see on "pehme koht", et lisada veel üks portsjon.

 

[Kylemalone1297]

What all am I looking for during the reaction, can u see when it is happening and when it is done ? Can u explain more about what the chemistry is behind what is happening during the reaction. Just to have more understanding of how it works

 

[WinterDust]

Tere,

Küsimus,

Kui amfetamiiniõli kristalliseerub väävelhappega, on aeg amfetamiini välja filtreerida Buchneri trummeliga, minu küsimus on järgmine. Millist filtreerimispaberit soovitatakse selleks kasutada?

Näiteks vaatan filtrit, millel on järgmised omadused, kas see on hea soovitus?

Filtri omadused:
Paberist valmistatud filterpaberid
Kõvad filtrid - filtreerimisaeg 140 sekundit (retentsioon> 2 µm). Aeglane filtreerimine.
Tihedad filtrid peente ja väga peente setete jaoks.
Kaal: 85 g/m2.
Paksus: 0,17 mm.
Filtreerimisaeg: 140 s.
Retentsioon:> 2 µm.

Lugupidamisega

 

[mile123]

1. Material:
Generally, tissue paper is not recommended for chemical filtration, especially in organic chemistry, as it may not provide the necessary chemical resistance and could introduce impurities.

3. Retention:
This retention level is suitable for filtering out larger particles, but if the amphetamine salt crystals are smaller than this size, they may pass through the filter. For crystallization processes, you typically want a filter paper that can retain smaller particles, ideally in the range of 1 µm or less.


4. Weight (85 g/m²) and Thickness (0.17 mm):
a relatively dense filter paper, which may be good for fine filtration but could also slow down the process. Thicker filter papers tend to have lower flow rates

Recommendations​

Quantitative Filter Paper:
Look for papers with a retention size of 1 µm or less, which would be more suitable for filtering fine crystals.


Buchner Funnel Filtration:
Whatman filter paper or similar brands that are specifically designed for vacuum filtration. These papers are available in various grades, including those with finer retention capabilities (e.g., Whatman Grade 1 or Grade 2).

src: chatgpt

Let me know if something is wrong

 

[ASheSChem]

hea küsimus... ka mind huvitab...
Tegelikult kasutan ma seda

aga ma ei tea, mis see on lol

ma nägin palju tüüpi filter "kvalitatiivne" või "kvantitatiivne" ja igas kategoorias versioon "aeglane" "keskmine" ja "kiire"...
mis on parim ?

 

[mile123]

Quantitative Filter Paper
Specification: 9.0 cm
The second image has a table with various specifications, likely describing different types of filter paper based on attributes like thickness, pore size, or filtration speed.

from chatgpt

 

[wannabewalter]

What is a purity of a final 60% - 70% yield? I found that there is such thing as amphetamine paste and amphetamine sulfate and sulfate is x2 in price. What is this final product (124.4g on video)?

 

[aaduo04]

a videóban a végső mennyiség szulfát. A paszta konzisztenciája tömeg szerint 3x lehet, mert az oldószerek nem párologtak el. (javítsatok ki, ha tévedek).

 

[G.Patton]

About 95%.

 

[Kylemalone1297]

Can I do a run of the synth with only 5g p2np ? To get a grip on it first.

 

[G.Patton]

You have to! Small scale batch is necessary to carry out several times before large one in order to understand this synthesis and remember it well.

 

[Kylemalone1297]

Is 5g p2np okay or too small ? And is pressure required during reaction or just the constant heating ?

 

[G.Patton]

Yes, okay. Atmosphere pressure.

 

[Kylemalone1297]

Is the pressure required or will it do fine just running hot with no pressure? Do I need to hold as much pressure as possible ? I have a nice 1000ml heavy wall round bottom. So it will hold some, but if it isn’t needed I won’t worry about it.

 

[GhostChemist]

Synthesis in this topiс without pressure (Atmosphere pressure)

 

[Ironbender]

I tried this synthesis on a small scale.
It failed completely. In the end I didn't even receive A-Oil.

This was my path:

p2np 10g

IPA/H2O (1:2) IPA 120ml/H2O 60ml (180ml)

NaBH4 17.4g

CuSO4.5H2O 7.9g in 20ml H2O

NaOH 25.6g in 80ml H2O

First water and then IPA were filled into the flask at room temperature and stirred.

NaBH4 was completely filled into the flask and stirred overhead.

p2np was added over a period of 30 min.
The temperature did not rise above 45 degrees.

When all P2NP was in the flask I increased the temperature to 55-58 degrees and refluxed for 40 minutes.

Then CuSO4.5H2O
dropped into the flask. Black copper immediately formed
Somehow the temperature didn't increase.

The RM was heated in a water bath to 78-80 degrees for 30 minutes.

The flask was left at room temperature for 1 hour.

There were 2 layers in the flask, black copper at the bottom. 'Amber cloudy at the top.

There was something slightly yellow in between that couldn't be dissolved.

Then 80 ml of 25% NaOH was added to the RM and a dark amber layer became visible.

It didn't smell like amphetamine base,
it smelled very flowery.
Nothing reminiscent of Amphetamine Oil.

Can someone explain what was wrong?
I followed the small scale instructions from this thread

p2np was from BM-chemistry
and looks very clean and bright.
It can't fail because of that.

I'm sorry for the bad English, hope you understand what I want to say.

 

[GhostChemist]

In original synthesis used CuCl2