Question AB Extraction question

[Cardboard1234]

I’ve followed the guidelines in AB Extraction and I’ve arrived at the end product. I’m not sure if what I have is correct as it does not look like the powder form end result as shown in pictures. Instead I have this gooey paste that I’m currently waiting to dry up. Does anyone know if this is normal? I’ve washed it with acetone already.

 

[G.Patton]

Hello, first of all make it dry. Looks as wet amphetamine. That's all.

 

[Cardboard1234]

Thanks for the prompt answer Patton. I did another batch and as I added sulphuric acid, after the solution stopped boiling, I got this layered solution, it looks different from the batch above. I followed the ratio of 1:1 of acetone and sulphuric acid. Do you know what this is? It’s Transparent on top, then red in the middle and orange on the bottom.

 

[UWe9o12jkied91d]

over-acidified

 

[UWe9o12jkied91d]

you may solve this with addition of naoh aq, sol. , extraction and reprecipiation (you will have losses)
add acid dropwise and stir

 

[Cardboard1234]

Thanks, I’ll try that. What sulphuric acid concentration do you use? I’m currently using industrial grade 99.8% so I probably won’t be able to use 1:1 ratio with the acetone to prevent this from happening again.

 

[UWe9o12jkied91d]

No clue, over 95 always in any case.Small scale u cant be very agressive with addition, it can go poof with just a few extra drops, dilluting your sol. with more aceton to acid 1:20 for example you can better control your addition.And give it time stir well before adding more again.
I like to suck back a drop or so of acid into pipette and suck over it some freebase sol, if it goes clear i take a ph reading, if it gets cloudy still I know I can add more.

 

[G.Patton]

>I added sulphuric acid, after the solution stopped boiling
Which solution do you mean? Explain in details please.

 

[Cardboard1234]

Thanks Patton, I’ll try that. What sulphuric acid concentration do you use? I’m currently using industrial grade 99.8% so I probably won’t be able to use 1:1 ratio with the acetone to prevent this from happening again.

 

[G.Patton]

1:1 Suitable for 99% sulfuric acid:acetone, pay attention to pH and temperature. High temperatures should be avoided.

 

[Cardboard1234]

I see, I’ll try using an ice bath while slowly adding the sulphuric acid on the next batch. Thanks for the insight. Do you know if the overacidified mixture is recoverable? The NaOH method does not seem to work produce any promising result.

 

[G.Patton]

You can try to extract it back as soon as possible by NaOH. You will loose part of amphetamine.

 

[Cardboard1234]

The mixture of amph free base + acetone, after adding sulphuric acid has a boiling-like reaction where the salt formed and started foaming bubbles.

 

[G.Patton]

You have to add the acid as slowly as possible and check pH of amphetamine mixture, you need 5.5-7 pH. No less. Probably you've added a lot of acid and too fast and burned (overoxidized) your amphetamine free base.

 

[HerrHaber]

it's much safer to add 1mL conc. H2SO4 to 25-30 mL's of acetone and carefully/slowly drop that with stirring to your freebase solution (part of which can be kept in a different container in order to add it in just in case you drop too much acid)

 

[chicaloca]

yes 1:5 with 'dry' acetone or IPA and keep 50% of the base in case you need it when over-acidified... (never personaly made it but on the road, hey...) and keep stirring 5 minutes before checking pH because it takes a little time to happen

 

[HerrHaber]

your statement already smells of success... it almost turns me on (just add the acid drop by drop with all the patience your love for chemistry has)

 

[sorena2316]

Hello, the correct amount is 1.10, that is, it should be ten times of sulfuric acid so that the color is not red. The easiest way to use 37% hydrochloric acid

 

[cokemuffin]

You have to use HCl gas to aquire dry amphetamine HCl, 37% will just result in a mess

 

[HerrHaber]

Ok, my bad then... when i started (well over a decade ago when I was a biochemistry undergrad) I was made to understand that the hydrochloride of this speciffic compound is by no means worth frustrating myself trying to make. I am well aware that for our common interst amines hydrochloride is the first thing to try (at least when performing preparative research on new materials)

 

[cokemuffin]

You're right, HCl salt is not worth it in the stated scenario, but you replied to a comment of me in which i only clarified that you can't use aqueous HCl or you'll get a mess and instead should use HCl gas for hydrochloride. For amphetamine the sulphate salt and specific phosphate salts are way superior, but my goal right here was just to correct the wrong information that kid is spreading.

 

[Cardboard1234]

Thanks for the tip guys, I’ll experiment around with different ratios and see what works best. I couldn’t find in the forum regards to how I can dry up wet amphetamines though. I’m thinking of putting the wet amphs in a sealed container separated with MgSO4. Would that work? I’ve tried drying it overnight in the room but it still looks wet.

 

[HerrHaber]

that is a dessicator what you describe... given that the MgSO4 is anhydrous it will work (if water is what you need to get rid of)

 

[G.Patton]

As @HerrHaber said, use Vacuum desiccator for your issue.