Amphetamine purification by acid-base extraction

[deeperdive36]

So I'm struggling with step 8. Seems like a lot of waste and loss for me here. I transferred extract from sep funnel added magnesium put in freezer. Now here I did the filter with vacuum. I think Buchner is way better than the setup I got as it leaked and volume is too large. So 1st when pouring into setup are you suppose to dump the whole thing in... I don't understand how to properly pour off the ether extraction without getting magnesium with it unless I don't pour all of the extract then at that point I have a lot of extract left with the magnesium what do I do with that remaining part to separate. Also I've attached pics of the leak. What do I do with this. Is this all waste . If there is magnesium that got through the filter what should I do? Basically stuck and waiting at this step

 

[Mr Good Cat]

Come on, man: you can do it. If me with my arms growing from my ass can, then you can too.
And yes! Nothing is more pleasing to my eyes than MDMA after ether washing.

 

[deeperdive36]

It's joanlab vacuum filter... It was cheap but the design is all wrong it allows stuff to leak on the outside... Ya I will try pours differently I read the sticky Patton wrote helpful in clarifying things a bit

 

[ACAB]

@deeperdive36 It looks like it is a ball joint which is held together with a clamp.
Have you tried greasing the ball joint with grinding grease beforehand and turning the ball until the grinding becomes clear?
That should solve your problem.

 

[deeperdive36]

Ahhh I do remember reading somewhere about greasing it. I will try it today hopefully will fix the problem. Thanks.

 

[Mr Good Cat]

@G.Patton general, does it worth to heat the water + FB solution + p.ether 40/60 up to 38-39C while ether washing is performed? probably it shall increase ether solubility and make emulsion dissolvation more easy?

 

[UWe9o12jkied91d]

You can wash with something less volatile, but I don't think it's worth to heat at all if it matters.

 

[G.Patton]

I think it isn't a good idea. You can add carry out two extractions one by one and add NaCl to the water in order to separate layers easier.

 

[Mr Good Cat]

Yes, you are right, NaCl works pretty well. I tried it a couple of times in proportions 15-20 gr : 100 ml and it makes my life much easier.
But still thinking, may be proper temperature can improve the process much better.

 

[G.Patton]

Carry out an experiment and figure it out.

 

[Mr Good Cat]

I did try ABE with liquid kept in the freezer.
There was 50 gr of salt that shall give 42 gr of FB.
Immediately as alkaline was added, the solution was put into the freezes for 4 hours. Then p.ether previously kept in the freezer too was added.
As the result, separation done much easier with 40 gr of FB in the result. But, the color of resulting FB was not pure transparent: slightly yellowish.
I mean, slightly yellowish - not pure transparent, but still acceptable: not cola

 

[Osmosis Vanderwaal]

I've just read this thread. I thought to myself, " why are we going to pH 12 with the NaOh?" We didn't go to pH 2 so it's not balanced. Then I remembered an experiment I tried using oil as my non-polar. When I neutralized the HCL with NaOh, what happened? I made lye soap. Petroleum ether has factions that react to make parrifin. That is what is going on here. The parrifin is the 3rd layer, pH 12 is overkill and petroleum ether reacts with sodium hydroxide. Correct me if I'm wrong, I'm not a chemist

 

[InLikeFlynn]

Should we evaporate 2/3 volume DCM like we do Ether in step 9?

 

[Mr Good Cat]

Another attempt of ABE.
About 300 gr of mdma hydrochloride at the beginning.
1.2L of water
85 gr NaOH
+ about 150 gr of NaCl lab grade added in process.

As NaOH added, pretty dirty black FB layer appeared in bottom layer (not top layer!!!), so i added NaCl to turn them over.

At first step 180 gr of perfect pure fb were extracted with p.ether, that is extremely low yeld.

Water leftovers left in the bottles for a week or something.

After a while, another step with 500 ml of DCM brought me 20 gr of slightly yellowish FB, that I would personally rate 9/10.

So, final yeld is 200 gr in total
Lost 50 gr

 

[curlyfries]

Its almost impossible for me to dissolve amf 1/1 in water. ( tried 2times with 2diffent bad batches).
Amf is from ai/hg.
- till what temperature can we heat 1/1 water/amf solution ? ( 80*c ?)
- howmuch extra water can we add?
waited like 1 hour to dissolve 20grams of impure amf in water with magnetic stirrer ( there were some chuncks in it, will make sure its extra fine next time) .
When i somehow try filtering the solids wich didnt resolved in water, the residue left behind in buhner filter is like muchy salt structure.

 

[InLikeFlynn]

Note: I’m using DCM as my solvent

When adding acetone to the reaction mixture on step 10, I saw 2 separate layers form and with the addition of sulphuric acid/acetone solution i was not able to salt any powder out of the reaction mixture.

What did I do wrong? Are there specific techniques needed when using DCM instead of ether?

 

[ActionAyi]

Thanks a lot i will try the first Method

I often did the Method 2 but i just filtered it with Coffee paper filtre and think with Acetone better results.

 

[garro]

First, ty to everyone sharing your knowledge.

Second, i fucked up the A/B extraction and need some advice on whether what I have is recoverable or not.

I'm using
1) Lye
2) Sulphuric Acid (Drain cleaner)
3) VMP Naptha
4) ~3g meth

Everything was going well. I extracted the freebase layer and froze to remove any water. Then I think I over acidified. I tried to recover it and caused more of a mess. I currently have two layers, one water(PH ~2) and one naptha There was also some particulate matter which has either been filtered out or dissolved in the water layer.

I also diluted the sulphuric acid with water, not acetone. I believe this was a mistake, please correct me if I'm wrong.

Few questions:
1) Is it possible to recover any product from this? If so what steps would you recommend?
2) In the future, If I over acidify, what should I do to recover the current process, or reset back to start (amph in distilled water)
3) Can I do the A/B w/o ether/spirits layer? As I understand the process, this would leave water soluable cuts, but just want to verify.

 

[EmilioE66]

Hello i have a question. Whats ideal PH for Amphetamin (liquid Form Mixed with methanol) when adding sulfuric Acid ? The Amphetamine 1:2 with methanol has ph 12.

 

[EmilioE66]

When the Amphetamin has ph12 i have to put sulfuric Acid Till it reachs ph 6 Right?

 

[kinkyfeet1]

Hi General Patton, I cant find any resource that shows the final production of the pink adderal pills. If i want to make the pink adderal pills, do i have to follow this instruction specific?Thank you for your time and help.

 

[HIGGS BOSSON]

Are you interested in the pink color or the composition of the admiral, which includes different salts of amphetamine and dextroamphetamine?

 

[kinkyfeet1]

Arent all adderal pills pink color on the market? sorry for my naive question, but i want to look into the production of adderal, and how can i start on that?

 

[kinkyfeet1]

I have taken one before and it was super helpful for me to focus. it was a pink pill and 20MG written on it I think. is there anyway i can produce the same thing at home or even in a lab with the right resources?