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

[Pervitin]

My syntheses still bubling after adition of cucl2 and refluxing it. Should I still vacuum destill the ipa of or wait ?

 

[Melv99]

I added a small amount of CH₃COOH to kill the Nabh4 before filtering.

 

[Pervitin]

thanks, I have now my RM at my vacuum destilation aparatus and the pump is running so hopefully no product is lost. ( hope -600 mbar is enough, more can't get) I will soon heat everything up. Can I use hydrochloric or sulfuric acid also?

 

[Melv99]

Keep us posted.. I was able to distil off the IPA and very miniscule amount of product came over with the IPA. Finally got to see the oil floating. Since I didn't have a vacuum working at the time I extracted with a NP. Worked just find.

Interesting though was the yellow-ish orange color thst remain in the NP.. it smelled very sweet which It made me wonder if that was P2P that didn't get fully reduced.

 

[Pervitin]

Yeah I vacuum destilled it at the moment. I have clear product in the receiver, just like ipa. My oilbath is at 70 C, but steam temperature is at 50 C. Hope I fuked something up, because my magnetic stirrer was not strong enough and now I have a clear layer on top and this hard sludge on the ground. I think I have to invest in a kpg stirrer next time.

 

[Pervitin]

O.K. I looked today at my beaker after the last time I tried to distill the ipa off and put it an a glass. I get a yellowish, alcoholic smelling liquid. Inside the beaker is now this hard black lump. My two questions are now:

1. Should I try to make the sulfate or distill it longer?

2. How I can get rid of the rock hard lump without destroying my beaker?

Thanks for any help.

 

[WinterDust]

Hi,

I don't understand, how can there be a black lump after you have distilled your amphetamineoil?

Didn't you extract the amphetamineoil after adding NaoH 25%?

Best regards

 

[Pervitin]

I followed the steps in the video and after adding CuCl2 you have to volatilize or distill the ipa off, via vacuum destilation, like you can see in my previous post. I think its a mixture of NabH4 and copper at the bottom. I added no NaoH to the solution.

 

[Loki12]

I believe this was already solved, read the whole thread, if I understand you correctly then what you have at the bottom is a mixture of borax crystals from the nabh4 and cucl2. I think it was even @ImOutAlso who solved this or he was the first to mention this issue.

Read the whole thread like I said already, you do not have to distill the ipa off, you can simply filter the solution after refluxing to get rid of the copper, then you base it and put it in sep funnel where top layer should form and bottom layer of organic, separate top layer, its better quality, bottom layer you can extract with small amounts of ipa to get some more base.

If you can't or don't know how to distill the ipa off, then leave it be, just add more anhydrous acetone than you would then salt out the amph via adding sulfuric acid dropwise, until like ph 8, filter what you got, place the rest of the ipa to freezer for second crop, once it's cold add more acetone to the ipa to counteract having too much ipa (mentioned in the thread also) to get more sulph to precipitate out (apparently only works with sulph), repeat salting, combine the two crops then dry off ipa, wash with acetone and dry again.

 

[Pervitin]

Yeah I have read the whole thread multiple times. But I think he doesnt have a hard black rock that sticks all together, so I cant get it out of my beaker and it sticks to the bottom. I decanted some of the oil today and droped some sulfuric acid in it. It fumes and crystals appear. I will now try some of it after drying it. I will heat up after that the hard mass and put NaOH in the beaker to get rid of this.

 

[WinterDust]

If your goal is to only produce amphetamine sulphate and not amphetamine then no.

You don't need to distill of the ipa, you just ad sulfuric acid to it directly, this way you don't need to dilute your sulfuric acid with acetone or ipa. The ipa in the amphetamineoil is more than enough.

The "rock" that you get is mixture between the NaBH4 amd CuCl2, after you ad the NaoH 25% it will dissolve in the water layer and become lumpy instead.

So all you need to do it decant the amphetamineoil, the first layer.

Then you add ipa and do second extraction from the reaction mass.

Mix it with the first amd discard of the black residue that is left.

 

[Loki12]

I performed this reaction a couple of times now, thanks for posting it. From what I understand, if the top layer is whitish, this is because of overcooling and the reaction should be brought up to like 50c when adding p2np, before cooling the reaction down and adding the rest?

Also, sorry if this has been answered already, but would it be suitable to dry off the wet amphetamine sulphate from IPA in a vacuum dessicator over sodium sulfate to get rid of excess moisture? I believe I read to not use carbonate, but can't find the exact post

Also would it be fine after washing the sulph with anhydrous acetone to do the same (dry it over sodium sulph in a vacuum dessicator)?

 

[WinterDust]

I only do large batches 500g+

But I keep my reaction mass between 48-53c.

When it reaches 48c I ad 15mL of P2nP then it reacts exothermic and warms up to 53c and I wait until it cools down to 43c takes about 7min and ad another portion.

When it comes to drying, switch from ipa to acetone in your washing process, because acetone evaporates x2 as fast as ipa.

I don't use dessicator, I first vacuum filter it as much as possible, then it becomes damp. So I spread it on a large piece of glas in room temperature amd put a large room fan 2meters away on slow blow. 1kg dries in a couple of hours. Oh yeah, you really need to have good ventilation for this since the fumes will stink as hell and they are igniateable.

 

[Loki12]

1. Do you still use cooling to keep your reaction at the range you said? When I add the boro my temperature barely goes up 2 degrees to about 20c, but when I start adding small amounts of P2NP solid form it spikes to 40c+ which is why I overcooled the first times I tried this.

2. From 15mL I take it you dissolved the P2NP, can I ask in what? You add it then via equalizer funnel or how?

3. I was under the impression that I have to add acetone to IPA then add conc. sulphuric acid dropwise to salt out the amphetamine sulphate? In the other post you mentioned there is no need for acetone?

So if I understand correctly, you salt it out of straight IPA that you have resulting from reaction mixture, then you take the wet sulphate, vacuum filter off the IPA and wash right away with acetone? You don't wait for the sulphate to dry completely from IPA before washing it with acetone?

 

[Loki12]

@ImOutAlso
Thanks for the reply by the way, I appreciate the guidance.
I am currently using a big ceramic sink that sits on the floor to dry the amph and it works fine for even 1kg, but the small amounts I have gotten so far from this reaction (have only done it small-scale), they sometimes turn a little red or slightly yellow when left to dry out completely. I wonder if that is the problem of having overcooled the reaction and having unreacted chemicals or exposing the amphetamine sulphate wet from IPA to air for 8h+?
This is about how long it takes to dry from IPA for me completely, then I dissolve in anhydrous acetone and filter, all the colors get pulled off and I end up with 100% white amphetamine that dries from the anhydrous acetone in matter of minutes..

 

[WinterDust]

Hi,

When you ad the NaBH4?

1. You first ad the water, then you ad the IPA here you start to mix the water with IPA for 30 sec. Then you ad all of your NaBH4 and continue mixing.

After 30 seconds tou can start adding P2nP in small portions.

Yes, I use cooling, I have made a schematic of my cooling in this post, go back in the thread and you will se my setup.

2. No, 15mL is my small spoon that I use, I do not dissolve my P2nP in anything it's just the sice of the spoon.

3. If you want to salt out your amphetamine straight from the reaction there is no meed to dilute your sulphuric acid since the amphetamine oil is already mixed with IPA and prevents it from overacidifying or burn.

4. Exactly, there is no need to dry it from IPA since once you wash the final product with acetone it will be drained anyway with the acetone and it will become wgite as snow.

Right now you are just putting uneccssary work into it, to dry it first, then dilute sulphuric acid and then wash it once more. Makes no sense, takes longer time and the results are exacrly the same.

I get 95% > pure amphetamine sulphate.

Best regards

 

[WinterDust]

Hi,

Your color problem.

If your amphetamine is yellow all the way through is means it's still dirty from the reaction mass and needs to be washed.

After washing when you dry it in room temperature only the surface of the amphetamine get's discolored, yellow first then it turns pink and finally red, this is only oxidaztion and nothing to worry about.

Once it dries and you crush it to powder it will all become white again and then you just vacuum seal it.

Best regards

 

[Pervitin]

My oil and the amphetamine is a little bit green/blue, I think from the CuCL2. Should I wash it with ethanol, because I read that the copper is soluble in ethanol/methanol? Is it usable for this?

 

[WinterDust]

This should not be possible.

There are two reasons for this, you didn't extract the amphetamineoil correctly from the reaction mass.

Or you over acidified with sulphuric acid which turns amphetamineoil green/blue.

Try washing it with acetone or IPA.

 

[UWe9o12jkied91d]

To me it sounds like incomplete reaction brought on by overcooling perhaps? Your final material can get a yellowish tint for 2 reasons: there is base indicating incomplete precipitation or there is unreacted raw material.You can fix with recrystalization from hot water+alcohol solution, a/b purification.Washing will not be sufficient to remove raw material contamination, it will fix the presence of base however.
Blue I’ll be honest I haven’t heard of ever but it is possibly indicative of
Red is another colour you don’t want to see, it is indicative of over-acid, and your product will burn the user.For this reason you need to take ph readings often, especially at the end.Vacuum filtration also helps pull off the solvent your product is suspended in, giving it less time to degrade.

my adise would be to push this reaction as much as it will go without overflowing.I gave this advice before, sorry if I’m repeating myself but you can skip cooling until 50 or so degrees, apply cooling in coldish water then just keep adding to keep your temp into as high range as possible.This way your temp keeps dropping due to water bath and you keep bumping it back up in a suitable range.Same with CuCl2 addition but you can turn it up higher if foaming is not issue.I would not skip reflux or at the very least remove cooling water in the end and let it go until it stops bubbling hard and comes back down to room temp.

 

[Loki12]

@ImOutAlso
I do exactly like you said in step 1, first water, then IPA, turn on stirring, make sure it is going nicely and then add all NaBH4. Temp rise is +1-2C.
I did see your setup, quite nice, I was also impressed by the equipment choice you described, definitely wish I had went the more budget route also.

The next time I finish salting out, I will vacuum filter off the IPA in the buchner and after stripping 99% of IPA, I will pour acetone on the moist cake, give it a stir and turn the vacuum on again, correct?

As for the color, I had read about oxidation of this compound years ago and your description confirmed it for me, it was in fact just oxidation

@UWe9o12jkied91d
Thank you as well, next time I will try cooling with cold water when it reaches 50C, I now believe I previously overcooled and way too early too, not letting the reaction reach the needed temperature. I add cucl2 dropwise dissolved in the least amount of water possible after adding the rest of P2NP and letting it stir for a minute or two.

When I apply the heat at 80C for 30 minutes, I am left with two layers, clear on top and blackish copper with nabh4 it seems like on bottom, but the reaction seems to still be going (bubbling) even after stirring is turned off and temperature is allowed to fall down to about 40C. I tried to solve this by heating for longer (50 minutes, it stopped refluxing at this point), but quite strong bubbling still persisted.
I read about this method and some people have mentioned this can be caused by unreacted NABH4 which is apparently added in excess in this synthesis, I believe they described adding acetic acid to "neutralize" the NABH4 and stop the mixture from bubbling, is this something that should be considered at all? Or is it fine if I run the reaction mixture through a vacuum filtration at 30-40C to get rid of boro and copper then proceed to base it with cold NaOH? I don't see any borate crystals forming when separating the layers, so I should be good, right?

 

[UWe9o12jkied91d]

My bubbling stops wholly once it cools down, say an hour or two after it’s left on reflux.
You may still be undercooling, give it some gas, be brave.

 

[WinterDust]

Yes,

When you wash with acetone, you don't need to stir, just keep the vacuum on and pour the acetone directly.