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

[diogenes]

You have to wash it by dry (without any % of water) cold acetone to pure white. Then, you can vacuum filter it and place in your foodbox into Vacuum desiccator or another chamber with vacuum.

G.PattonHi Patton, do you mean first vacuum filter off the IPA and then wash with dry acetone then filter off the acetone?

 

[G.Patton]

Hi Patton, do you mean first vacuum filter off the IPA and then wash with dry acetone then filter off the acetone?

diogenesYes. Also, you can wash with dry IPA as well. Acetone evaporates faster.

 

[diogenes]

Fantastic post, thank you Eidolon for sharing the knowledge of the old masters, it also clarifies the role of Cu in the reaction.

Add a saturation amount of common table salt (NaCl) to the water extraction, because it has a higher affinity for water the last load of amine molecules get pushed out of solution and will enter the non-polar layer.

Eidolon-UKThis is such a great idea, and I have never seen it anywhere else. Can this be applied to any acid-base extraction generally?

I know Ciphir, normally after conversion of the nitro to amine, adds glacial acetic acid until pH=4 to push the amine into the aqueous layer (any fizzing is the quenching of any excess NaBH4, use less next time). Strip off the IPA up to about 97C, then basify to pH=11 with NaOH, now steam distil with a wall paper steamer connected to an inlet into centre of reaction vessel.

This is the only part which i didn`t understand. If you push the Amine from the IPA to the aqueous layer then separate it again by steam, it seems like some extra steps and reagents used when the bulk of the Amine is already in the IPA, why not just simple distill it off together with the extracts? What is the upside of this?

 

[diogenes]

Yes. Also, you can wash with dry IPA as well. Acetone evaporates faster.

G.PattonThis brought up another question. Do you recommend drying commercial IPA as well? I haven`t been drying it as the bottles usually say 99.9%, but this might not be true or it can be hygroscopic. Thank you

 

[WinterDust]

Hi,

Did my second attempt today, and it went much smoother this time.



As you can see in the picture,

To the left you have the "waterlayer" after extraction with NaOH 25%, and to the right you have the amphetamine-oil, freebase, a-oil, what ever you want to call it.

In the waterlyer flask you can see about 5ml of A-oil that I could not extract, I mixed the waterlayer with IPA and extracted the ipa layer, unfortunetly my home made distiller did not work, too many joints to grease and to much hustle, in my opinion it's not worth the extra effort for a few extra ml.

I will need to invest in a rotovap later.

The amphetamine-oil was cleaned three times through buchner funnel and clean filters each time.

Let me know what you think.

Best Regards

 

[ElementalEnigma]

Hi,

Did my second attempt today, and it went much smoother this time.

View attachment 7353

As you can see in the picture,

To the left you have the "waterlayer" after extraction with NaOH 25%, and to the right you have the amphetamine-oil, freebase, a-oil, what ever you want to call it.

In the waterlyer flask you can see about 5ml of A-oil that I could not extract, I mixed the waterlayer with IPA and extracted the ipa layer, unfortunetly my home made distiller did not work, too many joints to grease and to much hustle, in my opinion it's not worth the extra effort for a few extra ml.

I will need to invest in a rotovap later.

The amphetamine-oil was cleaned three times through buchner funnel and clean filters each time.

Let me know what you think.

Best Regards

ImOutAlsoYou can add some non polar solvent to aid extraction.

 

[blackburn]

Hi,

Did my second attempt today, and it went much smoother this time.

View attachment 7353

As you can see in the picture,

To the left you have the "waterlayer" after extraction with NaOH 25%, and to the right you have the amphetamine-oil, freebase, a-oil, what ever you want to call it.

In the waterlyer flask you can see about 5ml of A-oil that I could not extract, I mixed the waterlayer with IPA and extracted the ipa layer, unfortunetly my home made distiller did not work, too many joints to grease and to much hustle, in my opinion it's not worth the extra effort for a few extra ml.

I will need to invest in a rotovap later.

The amphetamine-oil was cleaned three times through buchner funnel and clean filters each time.

Let me know what you think.

Best Regards

eyelowVery nice How big are your batch? And under how long time are you adding the P2NP for, to keep the temp under 60c ?

Best Regards

 

[WinterDust]

Very nice How big are your batch? And under how long time are you adding the P2NP for, to keep the temp under 60c ?

Best Regards

Sweswe
I am currently doing batches of 200g of P2nP.

I have quite good cooling method so my temperature never exceeds 47celsius.

It take 1h to add the whole portion of 200g.

Once you add the P2nP the reaction takes a little while to occur the first time, and it starts to foam, during foaming. Don't add more P2nP! Wait until the foam settles and you can see 60% foam and 40% liquid, that is the "soft spot" to add another portion.

 

[Gerald Cotten]

I am currently doing batches of 200g of P2nP.

I have quite good cooling method so my temperature never exceeds 47celsius.

It take 1h to add the whole portion of 200g.

Once you add the P2nP the reaction takes a little while to occur the first time, and it starts to foam, during foaming. Don't add more P2nP! Wait until the foam settles and you can see 60% foam and 40% liquid, that is the "soft spot" to add another portion.

ImOutHey man, can you tell me more about your cooling method? I am very curious.

 

[ASheSChem]

it until the foam settles and you can see 60% foam and 40% liquid, that is the "soft spot" to add another portion.

eyelowhi;
what about the AIluminium amalgam ? you prepare one for 200gr or 400gr?

 

[WinterDust]

hi;
what about the AIluminium amalgam ? you prepare one for 200gr or 400gr?

ASheSChem
You are in the wrong thread, there is no aluminum amalgam in this synthesis.

 

[G.Patton]

Do you recommend drying commercial IPA as well?

diogenesYes, I recommend to do it at least over MgSO4.

 

[WinterDust]

Question,

I am currently doing the following ingredient scale:

IPA 2:1, 3,6l
NaBH4, 348g
P2nP, 200g
CuCl2, 20g + 40ml H2O
NaoH 25%, 1,6l

I learned that the scale was linear so these are the measurements I concluded.

Now to the question, if I keep all of the ingredients at the same scale but only increase the P2nP too 300g instead, what would the outcome be?

Best regards

 

[WinterDust]

Hi,

Followup question, regarding amphetamine-oil.

Amphetamine-oil has a boiling point of ≈201⁰c

IPA has a boilingpoint of ≈84⁰c

Acetone has a boiling point of ≈54⁰c

If we are not using a rotovap, or a distillation setup with vacuum. Is it possible to boil of the IPA / Acetone using a hotplate?

Would this have an negative effect on the amphetamine oil?

Best Regards

 

[Netflix]

did you pick the oil from the vessel with a syringe or some other device?

 

[KokosDreams]

I am currently doing batches of 200g of P2nP.

I have quite good cooling method so my temperature never exceeds 47celsius.

It take 1h to add the whole portion of 200g.

Once you add the P2nP the reaction takes a little while to occur the first time, and it starts to foam, during foaming. Don't add more P2nP! Wait until the foam settles and you can see 60% foam and 40% liquid, that is the "soft spot" to add another portion.

eyelow
Thanks so much, that's exactly the info I was looking for.

What is the cooling method you got?

 

[G.Patton]

Would this have an negative effect on the amphetamine oil?

eyelowProbably yes, because amph free base can be oxidized by oxygen from air during heating on air for a long lime. The purity of amph salt would be less.

 

[Mystery_chemistry]

hello somebody did some reaction to methanol? I did on ethanol and now I have quite a lot of pure methanol and I wonder if the reaction will be successful too ...

 

[WinterDust]

Hi,

Question regarding my a-oil, please take a look at the picture.

After I finalized my a-oil I had no time to "crystalize" it to amphetamine, so I put it in the freezer overnight, when I took it out it had separated into two layer, the a-oil on top and the "gele" on the bottom. What is this gele liquid that I have?

I extracted the oil from it and left the gele in the flask and let it stand in room temperature for a few hours too see if it would "melt" but it doesnt melt, it just stays in gele like state.

My only guess would be that the the water and ipa had a chemichal reaction in the freezer and became some kind of gel, in return "purifing" my a-oil from impurities, but I'm just guessing here.

 

[G.Patton]

My only guess would be that the the water and ipa had a chemichal reaction

eyelowIt is impossible. Was your flask closed in the freezer? Have you added any desiccants before freezer?

 

[WinterDust]

It is impossible. Was your flask closed in the freezer? Have you added any desiccants before freezer?

G.PattonYes, I had it in my roundbottomflask first and closed the intake with a lid while I had it in the freezer.

No, no desiccants have been used.

 

[G.Patton]

Yes, I had it in my roundbottomflask first and closed the intake with a lid while I had it in the freezer.

No, no desiccants have been used.

eyelowActually, I have no idea what is it. You can extract amph oil from this "jelly" by non-polar solvent like IPA or ether/petroleum ether. Maybe amph was polymerized...