One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

[gcblin]

Can someone explaine this white layer at the bottom i finished adding p2np to nabh4

 

[WinterDust]

Can someone explaine this white layer at the bottom i finished adding p2np to nabh4

gcblinHi,

What do you mean by "Finnished adding P2nP to NaBH4"?

You ad P2nP to the reaction mixed with IPA + H2O + NaBH4.

The NaBH4 settles at the bottom of the reaction if you stop stirring it will "rock up".

Best regards

 

[gcblin]

Hi,

What do you mean by "Finnished adding P2nP to NaBH4"?

You ad P2nP to the reaction mixed with IPA + H2O + NaBH4.

The NaBH4 settles at the bottom of the reaction if you stop stirring it will "rock up".

Best regards

ImOutYeah everything was addet properly i was worried about the white layer, soon i will be finishing up will post result photos

 

[MadHatter]

Yeah everything was addet properly i was worried about the white layer, soon i will be finishing up will post result photos

gcblinYup, like the man said, it's borate crystals. Also, if you leave the rm cooling overnight for some reason, ice-like boric crystals will aggregate at the bottom. Like a small glacier. I got this on a massive scale at my first run and really wondered what i was looking at. Tested, and drew the conclusion it had to be boric crystals.

 

[gcblin]

The photo didnt load the first time

 

[gcblin]

So i finished gonna put it in the freezer for the night and filter it tomorrow, had a bit of problems with adding acid took a really long time to get it right. What happens when overacidified one 100ml batch was 5ph so i left it separate what can i do with it?

 

[MadHatter]

after several experiments I can say that any of these reaciotns involving more than 4-5 g:s og P2NP will require overhead stirring. What happens is that when water gets consumed by reduciton nad iPA gets boiled off, the borohhydride starts to reciitate at th ebotto of the flask. Eventually it will sto the agnetic stirrer, and without agitation more will cystllize quickly into a large white solid at the bottom, not doing ny reduction. Temp will go down, H2 evolution stop.
I broke up the solid cake manually and heated the mix to 60, swirling,, running the magnetic stirrer to the max and jabbing any bigger pieces with my glass rod, but they were very difficult to dissolve.
After I managed however, temp started rising again. I also added 10 more g:s of NaBH4 about 10 mins before hte CuCl2, and the reaction upon addition was vicious! I added 15 ml as fast as I could, with some overbubbling as a result. After that, the reaction ran itself at almost 80 degrees without the need for external cooling, In the end, I had o quench the reaction with external cooling to sleep. I then had three layers in the collecting flask; clear upper layer, thick cake of coper oxide and a lower, brownish red lig´quid layer, where the reaction was still ongoing. Bubbles were shooting uo through the oxide layer konstantly, and they still werein the morning. Now every liquid part had gone transparent though. The third layer now consists of a growing layer of borate crystals,.Coolong the flask seemed to worsen the situation, and tomorrow I will acidify the contents with HCl to pH2 and distill off all the IPA:. I'll then basify it to H10, and steam distill the freebase. Sep funnel, then acetone, tehn phosphoric acid to pH 7.
We'll see whaat I get. '

 

[WinterDust]

after several experiments I can say that any of these reaciotns involving more than 4-5 g:s og P2NP will require overhead stirring. What happens is that when water gets consumed by reduciton nad iPA gets boiled off, the borohhydride starts to reciitate at th ebotto of the flask. Eventually it will sto the agnetic stirrer, and without agitation more will cystllize quickly into a large white solid at the bottom, not doing ny reduction. Temp will go down, H2 evolution stop.
I broke up the solid cake manually and heated the mix to 60, swirling,, running the magnetic stirrer to the max and jabbing any bigger pieces with my glass rod, but they were very difficult to dissolve.
After I managed however, temp started rising again. I also added 10 more g:s of NaBH4 about 10 mins before hte CuCl2, and the reaction upon addition was vicious! I added 15 ml as fast as I could, with some overbubbling as a result. After that, the reaction ran itself at almost 80 degrees without the need for external cooling, In the end, I had o quench the reaction with external cooling to sleep. I then had three layers in the collecting flask; clear upper layer, thick cake of coper oxide and a lower, brownish red lig´quid layer, where the reaction was still ongoing. Bubbles were shooting uo through the oxide layer konstantly, and they still werein the morning. Now every liquid part had gone transparent though. The third layer now consists of a growing layer of borate crystals,.Coolong the flask seemed to worsen the situation, and tomorrow I will acidify the contents with HCl to pH2 and distill off all the IPA:. I'll then basify it to H10, and steam distill the freebase. Sep funnel, then acetone, tehn phosphoric acid to pH 7.
We'll see whaat I get. '

MadHatterHi MadHatter,

This is not true, I do 450g reactions in a 20l fbf with 8x60 magnetic stirrer and did not once have this problem.

Best regards

 

[MadHatter]

Hi MadHatter,

This is not true, I do 450g reactions in a 20l fbf with 8x60 magnetic stirrer and did not once have this problem.

Best regards

ImOutAnd yet you just said borates build up in the bottom of the flask. If they do so enough, of course they will disturb the stirring?
Overhead stirring it is for me. I already have the setup. Overall, I think vicious agitation is key to the success of this reax. However you choose or can.

 

[WinterDust]

And yet you just said borates build up in the bottom of the flask. If they do so enough, of course they will disturb the stirring?
Overhead stirring it is for me. I already have the setup. Overall, I think vicious agitation is key to the success of this reax. However you choose or can.

MadHatter@MadHatter,

Not quite, what I said was that you need to keep stirring during addition of NaBH4 if it STOPS then the NaBH4 will rock up and it will be difficult to get it stirring again, but it is possible.

I do however agree that overheadstirring would be more reliable and better, but in my case it's one component less, and no special two-/three-headed flask is needed.

Best regards

 

[WinterDust]

@MadHatter it sounds to me like the reaction is not done.

If you have a top layer of CuCl2 then you stopped your reaction to soon.

After boiling the reaction for 30min at 80c the cooperoxide layer should not be present but at the bottom of the flask mixed with the NaBH4, the appearance of CuCl2 should be ashy.

Also the amphetamineoillayer should not be red/orange but almost transparent, when you ad NaoH 25% it becomes bright yellow.


Best regards

 

[MadHatter]

No, you are partly right. I had to quench the reaction like I wrote, so there were still s´reactions going on. The oxide layer was not on top, it was a middle layer with the major part consisting of colourless product layer.
But the thing was, I had it in a reagent flask, and since bubbling was still ongoing from the bottom layer I left it in the bathtub with the cork unscrewed, In the morning, the flask was still hot, and the red/brown water layer was gone, replaced by copper oxide and borate crystals. So the reaction had been ongoing on a slow pace the entire night!
I have now filtered off the crystal clear top layer, I will acidify it, distill off the IPA, then basify it to pH10, add loads of water and steam distill the freebase.
I was so excited about it, and then my goddamn vacuum pump breaks down!
I actually never steam distilled freebase under normal pressure, but can you?
Won't part of it break down if I blast it with 100 C?

 

[WinterDust]

No, you are partly right. I had to quench the reaction like I wrote, so there were still s´reactions going on. The oxide layer was not on top, it was a middle layer with the major part consisting of colourless product layer.
But the thing was, I had it in a reagent flask, and since bubbling was still ongoing from the bottom layer I left it in the bathtub with the cork unscrewed, In the morning, the flask was still hot, and the red/brown water layer was gone, replaced by copper oxide and borate crystals. So the reaction had been ongoing on a slow pace the entire night!
I have now filtered off the crystal clear top layer, I will acidify it, distill off the IPA, then basify it to pH10, add loads of water and steam distill the freebase.
I was so excited about it, and then my goddamn vacuum pump breaks down!
I actually never steam distilled freebase under normal pressure, but can you?
Won't part of it break down if I blast it with 100 C?

MadHatterYou should post pictures of your reaction, will be much easier to see what is going on with it.

Best regards

 

[MadHatter]

Well, I feel I know pretty well what's going on with my reaction . And sorry, I don't have any pics at this time. What I DON'T know is if you can steam distill freebase without using vaccum, or if you will loose product from the high temp? Do you know?

 

[WinterDust]

Well, I feel I know pretty well what's going on with my reaction . And sorry, I don't have any pics at this time. What I DON'T know is if you can steam distill freebase without using vaccum, or if you will loose product from the high temp? Do you know?

MadHatterHi,

You can distill your freebase in a open container, but it is not preferable.

Amphetamineoil will oxidize from air and you will loose yield and quality, using vacuum distilation is much easier and safer for that matter because you don't have to worry as much about the fumes from IPA.

Best regards

 

[caesare.robot]

swim Granny used to try this method in 100g p2np/2L flask... magnetic stirrer didn't work and then it became different))) working with gloves and hand shaking gave a result of 40g Aoil after water distillation... and that are the good news...
bads are that grannys hands got burned with hot borates in ipa through thick lab gloves! lots of exhaust even via active reflux! be careful!
now granny is on vacation detoxing this method

 

[blackburn]

swim Granny used to try this method in 100g p2np/2L flask... magnetic stirrer didn't work and then it became different))) working with gloves and hand shaking gave a result of 40g Aoil after water distillation... and that are the good news...
bads are that grannys hands got burned with hot borates in ipa through thick lab gloves! lots of exhaust even via active reflux! be careful!
now granny is on vacation detoxing this method

caesare.robotIts not possible to do this synthesis in a 2l flask with 100g p2np!

 

[UWe9o12jkied91d]

swim Granny used to try this method in 100g p2np/2L flask... magnetic stirrer didn't work and then it became different))) working with gloves and hand shaking gave a result of 40g Aoil after water distillation... and that are the good news...
bads are that grannys hands got burned with hot borates in ipa through thick lab gloves! lots of exhaust even via active reflux! be careful!
now granny is on vacation detoxing this method

caesare.robotDo you look like michael jackson now?

 

[WinterDust]

Do you look like michael jackson now?

UWe9o12jkied91dThis is your moment, my man

 

[caesare.robot]

Do you look like michael jackson now?

UWe9o12jkied91dmercury, Freddy...(ll)

lol

 

[tucoXxX]

5 steps. the reactor contains everything, let's say about 21 liters of reaction mixture. 30 minutes external heating 30 minutes. at this moment, how to heat it from the outside? there is a heating stick inside, I don't think there is a unit outside that I can control. I lower the tank, 2* 10L flasks. two flasks. two heating jackets required? (30 minutes at 80 degrees). after separation it goes. I think there is a solution, the reactor does not need to be lowered. somehow I keep it at 80 degrees outside heat. but how?? xdxd

 

[WinterDust]

5 steps. the reactor contains everything, let's say about 21 liters of reaction mixture. 30 minutes external heating 30 minutes. at this moment, how to heat it from the outside? there is a heating stick inside, I don't think there is a unit outside that I can control. I lower the tank, 2* 10L flasks. two flasks. two heating jackets required? (30 minutes at 80 degrees). after separation it goes. I think there is a solution, the reactor does not need to be lowered. somehow I keep it at 80 degrees outside heat. but how?? xdxd

tucoXxXI honestly have no idea what you are talking about.

But if it is about how to maintain 80c for 30minutes with a reaction mass of 21l which would approx. measure up to a 1kg reaction.

You should probably use a heat mantle if you can't afford one the next step would be a hotplate that goes up to 550c.

Best regards

 

[tucoXxX]

this phase includes everything necessary. just heat it at 80 degrees for 30 minutes. but there is a magnetic stirrer, it has a hob sheet (this is also suitable). 6. now add 8 liters to separate layers. I don't think it's a problem from here on. thank you for your answer

 

[tucoXxX]

Bongo bongo

 

[tucoXxX]

these moments are even before the separation, that's why L is so big. I was a little confused by this external heating.