Amphetamine synthesis from P2NP via Al/Hg (video)

[HIGGS BOSSON]

Hi, I haven`t got Allihn condenser right now, is it possible to use another type? Or perhaps a fractionating coloumn (this one does not have cooling though). Does it leave to a lot of decrease in effectiveness?

diogenesOther types of condensers can be used, but are best suited for this reaction Allihn condenser

 

[Honolulu98]

First time and this came out. What do you think?

 

[brianvene1]

First time and this came out. What do you think?

Honolulu98Woww congratz man
Please tell me hows goes everything, amounts used, reaction time, lab/house gears used

 

[Honolulu98]

Woww congratz man
Please tell me hows goes everything, amounts used, reaction time, lab/house gears used

brianvene1
You have everything in the main post, just follow the steps. I had several failures, when I made the mixture in the flask with the aluminum and the 1-phenyl-2-nitropropene and others. The reaction was quite violent, it was my first experience with chemistry and the truth is that it scared me a bit. The substance remains very solid when I try to pass it through the strainer. I have weighed it and got a 55% yield on the main substance.

But I will leave it tonight to air and tomorrow I will weigh it again to see if the performance has been maintained before.

 

[Honolulu98]

How much could production be scaled with this method without hurting performance by 60%-70%?

What equipment would be needed? I would like to increase production to a minimum of 50g per cooking.

Do all components scale the same?

 

[Honolulu98]

What do you think of my first product? It is the first time that I work with chemistry and the truth is that in smell/appearance I am happy

 

[HIGGS BOSSON]

What do you think of my first product? It is the first time that I work with chemistry and the truth is that in smell/appearance I am happy

Honolulu98The product looks pretty clean, accept my congratulations. What challenges have you experienced? Maybe there are any questions?

 

[HEISENBERG]

I have weighed it and got a 55% yield on the main substance.

Honolulu9870% is a good yield

 

[Honolulu98]

The product looks pretty clean, accept my congratulations. What challenges have you experienced? Maybe there are any questions?

HIGGS BOSSON
Challenge as such was to take the first step. Then everything goes fine. Although the reaction when you pour the contents into the aluminum amalgram I have to admit it scares me a bit.

I will continue doing a couple more syntheses with these proportions and quantities to practice.

I asked a couple of questions a little above my post.

How much could production be scaled with this method without hurting performance by 60%-70%?

What equipment would be needed? I would like to increase production to a minimum of 50g per cooking.

Do all components scale the same?

 

[G.Patton]

Do all components scale the same?

Honolulu98Yes, congrats with synthesis!

What equipment would be needed? I would like to increase production to a minimum of 50g per cooking.

enlarge reaction flask and control temperature properly

How much could production be scaled with this method without hurting performance by 60%-70%?

as @William Dampier said before

Max quantity what I know was 2,5 kg P2NP per this reaction, but need good control for temperature. Gradual scaling of the reaction - the best choice. With any problems with scaling, it is better to solve them on smaller quantities. We can help on this path, with feedback.

Unfortunately, this reaction scales with a loss in yields. Optimally, I was able to load 100 g of phenyl nitro propene in a 20 L flask, with cooling in a basin with ice water, the solution of p2np in amalgam was added in 3 portions.

 

[Honolulu98]

Unfortunately, this reaction scales with a loss in yields. Optimally, I was able to load 100 g of phenyl nitro propene in a 20 L flask, with cooling in a basin with ice water, the solution of p2np in amalgam was added in 3 portions.

HIGGS BOSSON
I don't have much experience but a 20L flask and the amounts to use x10. Won't it be a bit tricky to handle manually?

What would it take? A rotary evaporator in an ice water bath?

 

[G.Patton]

What would it take? A rotary evaporator in an ice water bath?

Honolulu98Ice water bath and top stirrer. I showed the example, you can carry out 100g at first and enlarge your synthesis step-by-step to avoid spoiling reagents.

 

[cyb3r0]

0:04-0:40 - Preparation of an aqueous solution of alkali. In this video, it was made in advance so that the solution cools down by the time the main reaction mixture alkalizes. Alkalinization proceeds with the release of heat, and if a fresh hot alkali solution is used, then the exothermic will be more pronounced and forced cooling of the reaction mass will be required.

HIGGS BOSSONCan I use distilled water instead of alkaline water?

 

[HIGGS BOSSON]

Can I use distilled water instead of alkaline water?

cyb3r0No, because you need to alkalize the reaction mass

 

[cyb3r0]

This is a mixture of acetic acid, p2np and IPA, but a color appeared from this, why?
Knowing that the p2np was saved in the freezer? What do you think of the mixture?

 

[WillD]

This is a mixture of acetic acid, p2np and IPA, but a color appeared from this, why?
Knowing that the p2np was saved in the freezer? What do you think of the mixture?

cyb3r0p2np low quality or mistaken with other reagents

 

[diogenes]

I have been thinking what the right amount of Mercury nitrate is for amalgamation. I haven`t got Mercury nitrate or chloride so I have to use the nitric acid method, however the amount given in the video for Mercury nitrate synthesis is 5ml, which is about 25% of the Thermometer`s mercury content.

In the video which uses already made dry Mercury nitrate 0.1g Mercury Nitrate is given. This corresponds to roughly 62mg mercury. In the Mercury Nitrate/Thermometer video it is suggested that we use 1/4 of the total amount (5ml out of 20ml), which is at least 250mg Mercury if the thermometer contains 1gr. (normally mercury content is given between 0.6 and 3g). This is quite a substantial difference (X4).

 

[diogenes]

Another question. Can you `overdo` amalgamation e.g. by using too much Mercury nitrate? I have tried to make amalgam, but it somehow disintegrated, the whole thing happened very fast well under 15minutes and most of my foil became `sludge`. Any tips on how to spot the right time and how to make the reaction slower? Sorry if this is something very obvious, but I still managed to get it wrong, even if I was watching for signs like bubbles etc.

 

[G.Patton]

I have been thinking what the right amount of Mercury nitrate is for amalgamation. I haven`t got Mercury nitrate or chloride so I have to use the nitric acid method, however the amount given in the video for Mercury nitrate synthesis is 5ml, which is about 25% of the Thermometer`s mercury content.

In the video which uses already made dry Mercury nitrate 0.1g Mercury Nitrate is given. This corresponds to roughly 62mg mercury. In the Mercury Nitrate/Thermometer video it is suggested that we use 1/4 of the total amount (5ml out of 20ml), which is at least 250mg Mercury if the thermometer contains 1gr. (normally mercury content is given between 0.6 and 3g). This is quite a substantial difference (X4).

diogenesHave you found answers for your questions there Aluminium amalgam (Al/Hg) summary ?

 

[diogenes]

Have you found answers for your questions there Aluminium amalgam (Al/Hg) summary ?

G.PattonHi Patton, in a way yes, as you actually gave a proportion 1300:1 for Al:Hg, which roughly corresponds to the 0.1g of pure Hg(NO3)2 given in the video. On the other hand I still don`t know why fresh Mercury nitrate is given in a different proportion, or (another possibility) where my calculation goes wrong. That thread is very useful thank you for thinking of it.