P2NP'den NaBH4/CuCl2 ile Tek Kapta Amfetamin Sentezi (1kg ölçekli)

[SelfExper1menter]

Herkese merhaba. Bu tarifi kullanarak küçük ölçekte bir miktar amfetamin yapmaya çalıştım, ancak başarısız oldum. Her şey yolunda görünüyordu, kuruduktan sonra ürünüm bir miktar kırmızılık içeren beyaz bir toz gibi görünüyordu. Eğer amfetamin sülfat olsaydı (ki yapmaya çalışıyordum), verim %84 olurdu. Sorun şu ki, bu amfetamin değil.

Fizyolojik etkiler
20-30 mg denedim, kesinlikle stimülasyon vardı, ama aynı zamanda ateşe ve görünüşe göre bağışıklıkta bir düşüşe neden oldu: birkaç gün üst üste aldığım her iki seferde de solunum yolu enfeksiyonlarına yakalandım (ilk seferinde bunun bir tesadüf olduğunu düşündüm). Bunu alan başka bir kişi 90 mg'a kadar herhangi bir uyarılma yaşamadı, sadece biraz ağız kuruluğu yaşadı. İkimizin de uyarıcılara karşı toleransı yok.

Kimyasal testler
1 g toz 10 ml H2O içinde tamamen çözünüyor.
Bir test tüpünde ölçülen toz kütlesine fazla miktarda NaOH çözeltisi eklediğimde, yaklaşık olarak doğru hacimde amonyak kokan bir serbest baz elde ettim. Freebaz tabakasını ayırdım, CaCl2 ile kuruttum ve asit ile titre etmeye çalıştım. Sonuç olarak, serbest bazın molar kütlesini yaklaşık 171 olarak ölçtüm (ve amfetamin için 135'tir). Ölçümlerim çok hassas olmasa da, aradaki fark yalnızca ölçüm hatalarıyla açıklanamayacak kadar büyük.

Prosedürden sapmalarım
1) P2NP eklerken, bunun saatler alacağını fark ettim, bu yüzden sabırsızlandım ve reaksiyon şişesini oda sıcaklığında bir su banyosuna daldırdım. Bundan sonra P2NP'yi neredeyse tek seferde ekleyebildim ve karışımın sıcaklığı 40-50 °С'yi geçmedi.
2) Videoyu takip ediyordum, bu yüzden IPA'yı buharlaştırmadım ve doğrudan IPA / freebase katmanına conc. sülfürik asit ekledim.
3) O anda hiç asetonum yoktu, bu yüzden asitleştirmeden önce eklemedim ve filtrelenmiş "amfetamin sülfat" macununu IPA ile yıkadım.
4) IPA asetondan daha az uçucudur, bu yüzden çökeltimi sabit ağırlığa kadar kurutmak için birkaç saat fırına koymak zorunda kaldım. Fırındaki sıcaklık 80 °С'yi geçmedi.

Asıl soru şu: Nerede yanlış yaptık? Düşük verim veya hiç ürün olmaması beni şaşırtmazdı, ama amfetamin olmayan bir aminden iyi bir verim almak?!

 

[OrgUnikum]

The method as described here lacks all product workup/cleanup and and as such provides a very dirty and unclean Amphetamine, in special as NasBH4 reductions are all not giving very clean product. Purple MDMA and such.
I know the physiological effects like fever like very well and it is just the missing cleaning trust me.
There are several ways to do the workup, from distillation, normal, vacuum or steam of the base or dissolving the sulfate in water and washing this several times with toluene or petrolether or my favorite: 50/50 mix of petrol ether and Ethylacetate. Then evaporate the water and wash the resulting salt with copious amounts of Acetone and petrol ether as last. Already the simple washings give you a consumable product which does not make you sick like the crap which contains borate salts or else.

 

[w2x3f5]

CaCl2 amin ile kullanılamaz
1. İlk aşamada nitropropen, nitropropana indirgenir
2. amfetamin macununun bileşimindeki çeşitli tuzların safsızlıklarını aldı

 

[GhostChemist]

Chemical testing
The acid concentration must be precisely known (titration with standart solution of NaOH).
In the titrimetric analysis the concentration must be used only in equivalent concentration or normality or molality.
If one reagent is a weak acid or base and the other is a strong acid or base, the titration curve is irregular and the pH shifts less with small additions of titrant near the equivalence point. Indicators such as Methyl red or Litmus should give more accurate results
This method cannot be applied in this implementation

 

[aaduo04]

H! sizce bu bir çalışma prosedürü ve oranları mı? bu bileşenlerden yapay zeka tarafından oluşturulmuş bir yöntem. Cevaplar için çok teşekkür ederim!

30g p2np'den Feniletilamin Üretmek için 16 Adımlı Prosedür

Çözücünün Hazırlanması:
İzopropil alkol (IPA) ve suyu 2:1 oranında karıştırın. Tüm reaksiyon için yeterli çözücü olduğundan emin olun (yaklaşık 100-150 ml önerilir)

Sodyum Borhidrürün (NaBH4) tartılması:
Yaklaşık 6-7 g NaBH4 tartın (bu yaklaşık 0,15-0,18 mol'e karşılık gelir, bu da 0,15 mol p2np'yi indirgemek için yeterlidir, kabaca 30 g).

NaBH4'ün çözülmesi:
NaBH4'ü soğuk IPA/H2O çözücü karışımı içinde çözün. Hızlı ayrışmayı önlemek için çözeltiyi buz banyosunda 0-5°C'de tutun.

P2np ekleme:
Sürekli karıştırarak NaBH4 çözeltisine yavaşça 30 g p2np ekleyin. Karışımın rengi kademeli olarak sarıdan daha açık bir tona dönüşecektir.

Karıştırma ve Sıcaklık İzleme:
Nitro grubunun amine tamamen indirgenmesini sağlamak için sıcaklık 0-5°C'de tutulurken reaksiyon karışımı 1-2 saat daha karıştırıldı.

Bakır(II) Klorür (CuCl2) İlavesi (Opsiyonel):
Katalizör olarak 0,5-1 g CuCl2 ekleyin ve 0-5°C'de 30-60 dakika daha karıştırın. CuCl2 indirgemeyi katalize etmeye yardımcı olarak reaksiyonu hızlandırır ve ürün saflığını artırır.

25 NaOH Çözeltisinin Eklenmesi:
pH'ı yaklaşık 9'a getirmek için %25 NaOH çözeltisini yavaşça ekleyin. Bu, asidik yan ürünleri nötralize eder ve feniletilaminin serbest kalmasına yardımcı olur.

Reaksiyonun Tamamlanması:
Reaksiyonun tamamlandığından emin olmak için karışımın oda sıcaklığında (20-25°C) 30 dakika daha karıştırılmasına izin verin.

98 Sülfürik Asit (H2SO4) ile Asitleştirme:
pH 2'nin altına düşene kadar dikkatlice %98 sülfürik asit ekleyin. Bu adım, safsızlıklar organik fazda kalırken feniletilaminin sulu fazda tuz formuna dönüştürülmesine yardımcı olur.

Organik Fazın Ekstraksiyonu:
Organik ve sulu fazları ayırın. Organik faz yan ürünleri içerirken, sulu faz feniletilamin tuzunu içerir.

Feniletilamini Ekstrakte Etmek için Bazikleştirme:
25'lik NaOH çözeltisi kullanarak pH değerini 10-12'ye yükseltin. Bu, feniletilamini serbest amin formuna dönüştürecektir.

Organik Çözücü ile Ekstraksiyon:
Feniletilamini dietil eter veya kloroform gibi organik bir çözücüye ekstrakte edin.

Organik Fazın Yıkanması:
Kalan alkali ve yan ürünleri uzaklaştırmak için organik fazı distile su ile yıkayın.

Çözücünün Buharlaştırılması:
Organik çözücüyü bir döner buharlaştırıcı kullanarak veya vakum altında 30-40°C'de buharlaştırın.

Kristalizasyon:
Ürünü saflaştırmak için ham feniletilamini soğuk aseton kullanarak kristalleştirin.

Kurutma ve Depolama:
Feniletilamin kristallerini vakum altında veya bir kurutma fırınında kurutun, ardından uygun şekilde saklayın.

Önemli Potansiyel Hatalar ve Etkileri:
Uygun Olmayan Sıcaklık Kontrolü:
NaBH4 eklenmesi sırasında çözelti aşırı ısınırsa, indirgeyici madde hızla ayrışabilir ve bu da daha düşük verimle sonuçlanabilir.

Hızlı Reaktif Ekleme:
P2np veya NaOH'nin çok hızlı eklenmesi ekzotermik reaksiyona neden olarak istenmeyen yan ürünlerin oluşmasına yol açabilir.

pH Kontrol Hataları:
Doğru pH değerinin korunmaması, kısmen indirgenmiş bileşikler gibi istenmeyen yan ürünlerin oluşmasına yol açabilir.
Aşırı Karıştırma veya Yanlış Kullanım:
Aşırı karıştırma oksidasyona neden olarak istenmeyen nitro veya nitroso bileşiklerinin oluşmasına yol açabilir.
Kontamine Reaktifler veya Ekipman:
Kirlenmiş reaktiflerin veya ekipmanın kullanılması, istenen ürüne benzeyen ancak farklı kimyasal özelliklere sahip yan ürünlere yol açan safsızlıkları ortaya çıkarabilir.
Her Adım İçin İdeal Sıcaklıklar:
NaBH4 İlavesi ve İlk Reaksiyon: 0-5°C
p2np Eklenmesi ve Karıştırılması: 0-5°C
Reaksiyonun Tamamlanması: 20-25°C
Sülfürik Asit ile Asitleştirme: Oda sıcaklığı (20-25°C)
Çözücünün buharlaşması: 30-40°C
Kristalleşme: -5-0°C
Özet:
Yukarıdaki adımların dikkatle izlenmesi ve uygun sıcaklık, pH ve temizlik koşullarının korunması, farklı kimyasal özelliklere sahip olabilen ancak benzer görünen istenmeyen yan ürünlerin oluşumunu önleyerek başarılı bir feniletilamin üretimi sağlar.

 

[waltjr5858]

6 to 7 G of borohydride is not reducing 30 G of p2np all the way to the amine and the copper on top of it. There's a reason why a large excess is used and it's mainly before the first part where p2np is added to the borohydride.

 

[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.

 

[waltjr5858]

I know what you mean by the flowery smell but I can't tell you what it is. I have had that exact failure. Even using cucl2. The copper didn't cause your failure... it's something else.

 

[waltjr5858]

But I do know that no matter what amounts are used as long as you either scale down or scale up preferably from the original video that is up on this site there is a caption that comes up during the video that says you should add the p2np over the course of 6 hours. The only time this reaction has really worked good for me with very strong effects at the end except was still dirty and needed proper cleaning but it worked. Normal stuff water alcohol and borohydride all together and then I took whatever I was using at that time for the substrate p2np and divided it by 24. Whatever that equaled that's how much I added every 15 minutes until it was gone which was 6 hours. I noticed on the last addition that there was no reaction from the nabh4 fornsome reason? Guess I used it all up possibly so I added a half a gram of borohydride just in case. Waited 5 minutes and started dripping the proper amount of cucl2 in. When doing smaller reactions it's really hard to tell if you have added copper until the black particulate stops forming because the flask is small to begin with and the whole damn thing turns black. So as according to the video they used 25 or 26 G to 250 g of p2np so I did a 10 G reaction and it was somewhere around a gram or a little over of copper so I just dripped the entire thing in. Once I was done adding I just cranked the heat until I hit 80c and waited about 35 minutes and allowed it to cool to room temperature and it worked perfect minus being completely contaminated with some kind of Borate.. once I noticed that I just redesolved and acidified to a pH of 3 gave it a wash with nonpolar and then refreebased and gave it a little water wash. Dried it and re-added acid to crash out... it is a finicky reaction and definitely not as easy as most people put it there has to be some kind of trick as to the temperature you put your copper in the reaction or how long to let it react before adding the copper or something there's a trick to make it consistent because I can definitely tell you the aluminum Mercury reaction is very inconsistent even worse than this one

 

[Tamishea]

Hello everyone. Im finished my first synthesis but i dont know that i do everything properly, when cooper black showed at the bottom i leaved everything at 75c and then after 30 min refluxing without Boiling because of temp 75c i have filtered thru coffee filter, and not leaved to room temperature and just added then 25% naoh. The layers are separated but the oil smells only IPA. And react with h2so4 but everything is green and pH Get down to 1,3. Should i take the temperature higher to 80 when black cooper is at the bottom and wait that smell from ipa is gone (evaporating with or without reflux condenser?) then leave to Room temperature AND THEN FIRST BASIFY WITH 25% NAOH? Please help

 

[GhostChemist]

``Should i take the temperature higher to 80 when black cooper`` - No, temperature before 80C or low (this stage more applied for big scale synth and help to evaporate IPA), as a variant for small scale synth 30-50 min at temperature 40-60C

 

[Tamishea]

When i give whole CUCL2 we say at 60c one hour long, then should it smells normally then? Because my synthesis give me yellowish oil but with STRONG smell from ipa and when i give sulfuric Acid it becomes greenish.

The scale was
300ipa 150 dh20
43,5 nabh4
25g p2np
2,375 cucl2*h20

 

[William D.]

I think these are the remains of reaction products. To avoid this, it is better to dilute the reaction mixture with water and extract for example with ethylacetate. After extraction, rinse the organic layer several times with water and acidify. Then there will be no excess color or burning when using.

 

[waltjr5858]

Absolutely. Something green? Either left over from condensation or which I still would not know what that would be or there is copper in the IPA. I have had copper in a certain form get either through the filter or whatever it got in there and it did turn slightly greenish bluish just like it is before when you make it up. This reaction to me is just hit or miss. It's definitely novel and I have had many many failures. Now p2np to P2P and then leuckart has always produced every single time. I still occasionally play around with the borohydride but it can be a pain in the ass. Or I have just tossed it in with LiAlH4 and called it a day. Hopefully that might give the person before that is having issues with the borohydride reduction to try something else they're still having problems instead of wasting precursor. Unless they have a bunch of it then who cares.

 

[mile123]

Hello!

When preforming vacuum distilation of ipa (step 8) , what vacuum pump to pick, if it is rated 10 000mbar and I need only 60mbar, is it possible to regulate it or I should buy rotary vacuum pump rated to 100mbar.


I found out that best range for ipa evaporation is 50-100mbar which is considered low vacuum, did anybody have experiences or suggestions with this problem?

 

[William D.]

Do not forget about productivity in liters. It may be that you use a powerful pump and it will destroy your filter. But a high vacuum can be used. 60mbar is more than enough for filtering.

 

[waltjr5858]

You will actually be surprised you do not need a very powerful pump and determining what suction you are running at is a pain in the ass. I actually have a very good vacuum gauge that I hook directly up to my system and test boiling temperatures of known substances and it's still a little all over the place. I think the best thing you can do is steam distillation If the product allows because it does come over nice and clean and then just dry it with potassium carbonate and you are in business. Definitely do not buy a rotary vein vacuum pump because I have destroyed probably five of those things. They are very powerful and I can boil water below room temperature easily but without inexpensive setup I do not have a way to regulate vacuum pressure. If you crack open a small leak on purpose to lower the pressure what that causes is air now flowing through the system instead of sitting at a vacuum which causes your product to go right into a trap or right into the vacuum pump and gone. Any kind of oil that can be steam distilled is absolutely worth the time it takes. If you definitely need vacuum they sell some on Amazon and they are called diaphragm pumps I believe and require no oil so there's no way for you to contaminate the vacuum pump when you do distillation. Just pump away and they definitely go low enough to let's say take a 200° C boiling temp and get it close to just a little over 100 so plenty low enough and definitely worth it over the rotary vein. I think they cost just a tiny bit extra nothing crazy. That was probably the best purchase I ever made as a vacuum pump after blowing up five of the other ones

 

[mile123]

Thank you for answer. You have a lot of practice and you confirmed my every doubt about vacuum distillation and provided more information than I could find on whole forum.

I also agree that rotary vein vacuum pumps aren't suitable since you have vapors, even with cold trap, it is cheaper to buy diaphragm pump.

I researched a lot about controlling vacuum, measuring pressure, but I think it isn't so important as maintaining right temperatures during process. In my head it seemed important.
My idea is to take fridge compressor from junkyard 600w, 20l/min and convert it into vacuum pump, then just test the theory, can I turn it on, and leave it running or reach maximum vacuum and then turn it off and see how it goes and how long it will last. I also hope that I don't need to do overhead stirring while vacuuming, but even if I have, I will get batch chemical reactor with everything on it for vacuum distillation and whole process.

I believe you about steam distillation, but I want to stick with vacuum distillation since large chemical reactors (200L) are designed to work well under vacuum and I don't have strength to do in depth research about steam distillation.

I will try and let you know the results, I may preform simple distillation just for start, to test final product.

 

[mile123]

I'm not sure if you saw this video , A Vacuum Distillation Unit, where he also didn't really care about boiling points and pressures, he just turned it on until process is done, there is also vacuum depth controlling tap but I believe it doesn't make difference in terms of control?

 

[William D.]

Vacuum diaphragm pump with PTFE membrane. I think the best for our tasks.

 

[mile123]

Yes, I agree with you, those pumps are worth of investment since you can apply them on large chemical reactors as well.

I just want to wait before purchase to see if I can carry whole process even with simple distillation.

 

[mile123]

One more question, has anyone tried this venturi water ejector, it works by putting pressure and ability to create vacuum and transfer liquids or gasses.