Синтез на амфетамин от P2NP с NaBH4/CuCl2 в едно гърне (мащаб 1 kg)

[Uncle Lee]

Тази реакция е много добра в малък мащаб
При голяма реакция опитите да се контролира екзотермата и голямото количество пяна чрез бавно поставяне на разтвора на CuCl2 в колбата няма да дадат висок добив, може да има само нитроалкани и концентрацията на наночастиците ще бъде твърде малка, за да се намали нитрото, трябва да се използва възможно най-голямата колба и целият разтвор на CuCl2 да се добави наведнъж

 

[waltjr5858]

But when you add all of the cucl2 at once the whole mixture turns black and then within minutes the catalyst falls out of the alcohol and doesn't do much down low... adding drop wise allows a continuous supply of copper to stay in the upper layer acting as a catalyst. So far I have found if you have too much nabh4 left at the time of adding the copper the copper gets reduced wayyy to fast and losses its catalyst activity instead of almost starting as a yellow or brown mixture and slowly turning black before finally falling to the bottom. Thise are the reactions that really work for me when the borohydride amount is low enough to not instantly reduce the copper to black and need the temperature increase to finally cause it to be fully reduced and settle in the bottom slowly over time.... but trying to get the perfect amount of nabh4 at that moment is let's say.... very difficult. Surprisingly the nitro doesn't need much nabh4 in the end to reduce.

 

[Mclssmxxl]

Гореща плоча, нагревателна мантия (може да е твърде много дори на ниска степен), дефо не открит пламък.

 

[Johnny Ringo]

Was ist die beste low budget alternative zu einem 600€ heizmantel?

 

[btcboss2022]

100% съм сигурен, че в грамите от следващата партида ще направя снимки. Получих 254 грама фребаза от 287 грама P2NP.

 

[Johnny Ringo]

Wie viel war es in flüssiger form?

 

[Montecristo]

Не получих много утайка от сол, когато добавих фосфорна киселина на моята 67-грамова партида p2np.
Ще се промени ли това по време на замразяването? мислех, че съм следвал доста добре инструкциите.
След като приключи добавянето на p2np, направо ли преминавате към cucl или трябва да изчакам да спре да реагира?
Разклатих я след добавянето на лугата и я оставих за около час, а при екстракцията с ipa я оставих да се отдели и след това отново я разбърках 3/4 пъти.
Дестилирах във вакуум ипа при 50-60oC , дали това е твърде горещо?
може би съм го подкиселил твърде бързо, тъй като в моята сепарираща фуния все още имаше воден слой ( за всеки случай правя 2 екстракции с ipa), затова използвах спринцовка и не беше точно на капки..
някакви идеи? ще дам актуална информация, след като престои една нощ във фризера.

 

[Johnny Ringo]

Habe es auch versaut beim ersten mal gucke grad nach lösungen und schließe mögliche fehler aus. Hat sich bei dir auch nur ein kleiner teil umgewandelt und es ist größtenteils flüssig geblieben?

 

[pekonias]

Was your freebase purified? This reaction produces quite alot by-products so it's absolutely required to steam distill the freebase. Put 1ml freebase oil on petri dish and let evaporate. If the residue is not white it's not pure. If it's not pure and you turn it to salt, your power doesn't dissolve in water easily and yoy'll get sick if you take it.
So this was the boiling temp in the flask or bath temp? Not sure if too hot when I did it the BP was ~38 C while the water bath was kept < 60 C. (The BP only depends on pressure so higher bath temp. only makes it boil more violenly at same temp.) Do normal distillation of your vacuum distillate and see if anything solid remains in boil flask.
Might be dissolved in the water in it.

 

[Johnny Ringo]

Good to know the destillation is essential for this process thanks. I kept the oil and will try to purify it with destillation and see what comes out.

 

[Mclssmxxl]

Чух от Патън тук, че трябва да я загреете преди това. нещо, което никога не съм правил със сярна, но от друга страна, моята киселина е доста чиста.
Поръчайте от Полша, ако сте в ЕС, те ще ви продадат варели с буквално всичко lol

 

[Johnny Ringo]

Darfst du mir hier verraten woher du die schwefelsäure beziehst oder muss ich dir privat schreiben? Habe grad probleme welche zu beschaffen nur phosphorsäure iaz für mich aktuell laufend zugänglich.

 

[G.Patton]

Hello, if you wanna get answer, use English in this section please. You also can post your questions in Germany section in your native language.

 

[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]

I have question about vacuum distillation.

In order to achieve vacuum, my compressor has to run all the time to create good vacuum and tight sealing.

1. Is simple distillation with flask and reflux condenser fine or should I use fractional column like in alcohols, although in this video simple is enough

2. Does your IPA evaporate through vacuum pump instead in receiving flask since all air is sucked through vacuum out because unit runs all the time?

3. Why flasks need to be round bottomed, I have erlenmayer flask as receiving and I don't see reason why I should replace it with round bottom?

4. I also created moonshine, can you tell how to dillute % of ABV, water or distilled water makes it look less crystal clear.

Thanks

 

[dobrytowar55]

Hi. Can someone tell me what the cost of ingredients and equipment for producing 1kg is? I would be grateful if someone could tell me if it is enough to scaling up everything to get a larger amout or does that cause any discrepancies? Also can someone tell me what is the CAS of this final product?

 

[GhostChemist]

Find it in our Comercial Section

 

[OneTensionSkyRed]

It would be really REALLY great if someone could run a TLC analysis of the products from this reaction. I've read that NaBH4/Cu reduction mainly produces N-hydroxylamines instead of amines for alpha-alkyl nitrostyrenes. Because of similar melting points for their salts and similar boiling points, the only way to separate and identify N-OH-amphetamine is by chromatography. The N-OH product is also active as a stimulant but it is different to amphetamine. I wonder if this is really true.

 

[GhostChemist]

what source reports this information?
all compounds tested with qualitative and quantitative analysis
N-OH group can be formed as an intermediate compound if the experiment is not carried out correctly

 

[OneTensionSkyRed]

Yes, I should have probably researched this a little more before posting here, apologies. The source for this comes from amateur chemists and there aren't any official publications to support this

 

[Chemical Dream]

Is so much NaBH4 really necessary or is it excessive

 

[mile123]

Vacuum distillation can be avoided, final product may contain IPA, without NaBH4 you can't get final product at all. It is base ingredient along P2NP

 

[keras]

So. You get this pure amphetamine. How much would you cut it ? 1kg amph turn to 2kg ? Because amph cheap profit should come from cutting it or I am wrong?

 

[GhostChemist]

Our team is study science methods for obtain only pure individual substances. We do not support and do not give recommendations for dilution this compounds to increase mass, yields

 

[malignoalfa]

resultado de FTIR e GC-MS de amostra deste método.

 

[mile123]

Am I the only one who sees a lot of impurities here?

 

[adhdcurse]

Hello Guys. Can someone please post here what chemicals exactly form in each reaction, step by step. I am trying to understand each step. There are several steps where it is not documented what chemicals are actually created. I am trying to use a Chemical Reaction Simulator/Modelling Software, like Aspen Plus, HYSYS, COPASI, Chemcad, Matlab, Cantera, COCO etc.