The simplest Methamphetamine synthesis from Amphetamine

[G.Patton]

it's a vacuum filtration or a vacuum distillation (if this, how many temp C°?)

ASheSChemHello, "concentrated in vacuum" means that an amount of solvent is decreased by a rotary evaporator.

"dried over Na2SO4 or MgSO4 anhydrous." Means that you have to add one of this substance to collect all water from an organic solution. Look at here drying manual.

and.. this result is ... ? pale yellow methamphetamine (liquid? powder?) the one you use for ice?

methamph freebase liquid at room temp

sorry but i never done this before so... i'm a little lost

can I use this assembly for example?

Spoiler: photo

View attachment 7149

so... i put the "organic layers with methamphetamine (4) combined" (and my MgSO4? or in the 500ml one...?) in the 2000ml balloon ... and.. i put how many temp ? all the distillate is retained?

You don't need distillation setup, I didn't mention it in "Equipment and glassware:"

 

[ASheSChem]

thanks guys

Hello, "concentrated in vacuum" means that an amount of solvent is decreased by a rotary evaporator.

"dried over Na2SO4 or MgSO4 anhydrous."

G.Patton
so if we don't have a rotary evaporator (you say it's optional in equipment and glassware) ; we just dried over Na2SO4 or MgSO4 anhydrous?

 

[G.Patton]

we just dried over Na2SO4 or MgSO4 anhydrous?

ASheSChemYou have to evaporate solvent in any case. Rotovap is the best way to do it because you can collect evaporated solvent. You can use warm water bath for this purpose but you'll lose a solvent, also you need well ventilated workspace.

 

[ASheSChem]

You have to evaporate solvent in any case

G.Patton
maybe we can use this ?

 

[G.Patton]

maybe we can use this ?

View attachment 7153

ASheSChem

you'll lose a solvent

Chinese rotovap not so expensive. You'll use it quite often and save a lot of solvent. Also, you can use it as distillation setup for recuperation.

 

[MadHatter]

maybe we can use this ?

View attachment 7153

ASheSChemThose are not great for evaporating solvents. The evaporated solvent will just go into the pump and out in the air in the room. Since you're using flammabel solvents this can be really baaad, mmkey?

The earlier setup you posted is better: just a vacuum distillation of the solvent. Also, it recovers the solvent used. This is basically what a rotovap does, but without the rotation.

 

[ASheSChem]

okay okay
thanks to you both... now I better imagine the result that I should obtain...



now i need to understand step 7 lol

 

[G.Patton]

now i need to understand step 7 lol

ASheSChemThe HCl gas bubbling procedure was shown in one video tutorial (DET synthesis).

 

[ASheSChem]

The HCl gas bubbling procedure was shown in one video tutorial (DET synthesis).

G.Pattonthanks again!
I will be studying all of this over the next few weeks.

 

[teodor]

hi.i did the whole process on a small scale.i ended up with a yellow oil.is this methamphetamine

 

[diogenes]

In the original Rhodium article it's described as stereospecific:
"70g d-amphetamine in alcohol with aluminum and 1 mole formaldehyde gave d-methamphetamine, which was converted to the phosphate salt. 1-Phenyl-2-aminopropanol similarly yielded ephedrine."

MadHatterHi, this means that Rhodium recommends different proportions, an excess of formaldehyde? In the original text it says one-mole A and 1 mole formaldehyde. Is it worth doing it with the excess just in case?

 

[diogenes]

Has anyone seen a report using NaBH4 instead of Al/Hg to reduce the Imine in this synthesis route? Is there any problem with changing the reducing agent? Perhaps not compatible with the formaldehyde?

 

[primitiveintelectual]

what is the final yeld?

 

[G.Patton]

so... i put the "organic layers with methamphetamine (4) combined" (and my MgSO4? or in the 500ml one...?) in the 2000ml balloon ... and.. i put how many temp ? all the distillate is retained?

ASheSChemIt means that you have to dry your combined organic layers with MgSO4 (get rid of water) => filter solid MgSO4 after this => evaporate DCM and get methamphetamine free base. You don't need distillation apparatus for small scale synthesis. DCM can be evaporated in warm water bath easy.

Do you understand?

 

[ASheSChem]

Do you understand?

G.Pattonyes; thanks master

 

[finch3523]

"Imine (3) was reduced for approximately two hours, to keep reaction temperature below ~50-60 °C. Cooling should be applied if the reaction becomes too violent."

How you reduce for approx two hours? What does that mean? You just throw it all together and wait two hours or is there a special apparatus needed?

"Organic layers with methamphetamine (4) are combined, concentrated in vacuum and dried over Na2SO4 or MgSO4 anhydrous."

After this step you get freebase?

 

[UWe9o12jkied91d]

"Imine (3) was reduced for approximately two hours, to keep reaction temperature below ~50-60 °C. Cooling should be applied if the reaction becomes too violent."

How you reduce for approx two hours? What does that mean? You just throw it all together and wait two hours or is there a special apparatus needed?

"Organic layers with methamphetamine (4) are combined, concentrated in vacuum and dried over Na2SO4 or MgSO4 anhydrous."

After this step you get freebase?

finch3523Yes, it just means keep maintaining the reduction reaction that happens.Watch alhg amalgam video for p2np to get an idea of what it looks like and how it reacts, this is pretty much the same thing.It's not as simple as throw in the pot and do nothing, the mass expands, heats up rapidly, generates a lot of vapor etc. You have to apply cooling by immersing you reaction vessel in a water or ice bath juuust as long as it's needed to keep it from going out your condenser or 50-60 C like procedure recommend.If you don't have stirring you may want to swirl manually so reaction is more complete => bigger yield.
Yes, there is also no need to concentrate it under vaccum if you have a reasonable amount of solvent or alternatively you can steam distil which is more reasonable to accomplish for you I presume.Yes, the organic layer contains freebase.

 

[finch3523]

ah ok I need reflux condensator.

some more questions:

so there would no heating device be needed, the reaction will generate enough heat? Only cooling would be needed?
what temperature would be to low, because it sounds the reaction can stop?

If you have a round flask with three openings, how will you accomplish the stirring? If you have reflux condensator attached how can you do stirring?

will you mix amphetamine base and al/hg all at once or slowly drip the amphetamine base into the flask?

how much boiling chips you add?

after the two hours shoud you heat the solution in water bath to 50 Celsius for 30 minutes like in the amphetamine synthesis for bigger yield?

a 2 liter flask will be good if you use want to do 5 to 10 grams of end product? or maybe only 1 liter? can the reflux condensator be smaller than 5l?

do you need buchner flask with vacuum, can you just use coffee filter and fan?

Is separatory funnel needed, can you separate with syringe (plastic?), or will that not work?

how does the last step work with solvent work if I dont want to do steam distillation (I guess you would need additional apparatus for that). What would be the result .... methhcl?

 

[finch3523]

will the use of dex-amphetamine with this route result in d-meth? somewhere I read that if you use formaldehyde you will get racemic meth at the end?

 

[diogenes]

will the use of dex-amphetamine with this route result in d-meth? somewhere I read that if you use formaldehyde you will get racemic meth at the end?

finch3523If you use D Amph to start with you get D meth. I was planning to try this synthesis, and I plan to use racemic amph and then resolve the meth just in case something goes wrong with a route I have never tried, then D amph would be wasted...

Is there anyone who has actually tried this synthesis in practice? I have read it in several places, but never found a practical report. Experts can you please give some reassurance?