There is a problem with the synthesis of methamphetamine from amphetamine. Please help

[wael gano]

I started with an amphetamine base. The color of the free base was like amber after the solvent evaporated
Amphetamine base 3 grams
Formaldehyde 3ml
Alcohol IPA 12ml
With aluminum amalgam
Add the ingredients and heat for an hour and a half
After finishing, I added water and filtered out the excess aluminum
I added hydrogen chloride gas, pH3, and extracted with Dcm. The color of the extraction was yellow
After that, alkaline was added and extracted again with Dcm
The collected extracts were pink in colour
I evaporated Dcm, added ethanol, and pumped in hydrogen chloride gas, pH3. The color became pink, and I evaporated the ethanol until it became a red sticky substance.
I washed it with Dcm back salt
I melted the salt at a temperature of 180, and smoke appeared, smelling like amine, like the smell of amphetamine base. I don’t know.
The salt then turned a burnt brown color
Please I don't know if this is meth or something else

 

[wael gano]

After interacting with amalgam
Dcm extract colo

r

 

[wael gano]

After pumping hydrogen chloride gas to react amphetamine with formaldehyde

 

[G.Patton]

Hello, why do you pumped HCl gas to react amphetamine with formaldehyde, sounds like nonsense

 

[wael gano]

The translator made a mistake in writing
I did not do that
I mean this picture, after the acid-base extraction and the second alkaline extraction, I had a free base in Dcm solvent, its color was light yellow, and I pumped hydrogen chloride gas to it, and the color became pink.

 

[wael gano]

After evaporation of ethanol

 

[Mo0odi]

@William Dampier

@Marvin "Popcorn" Sutton

@G.Patton

@HIGGS BOSSON

@GhostChemist

I want to try this method


Does anyone know what happened in this experiment?

 

[G.Patton]

First of all, are you sure that your Al amalgam was okay? Do you have picture of it? Because it sounds like your amalgam didn't work.

 

[wael gano]

Amalgam is good
I mixed the base, ethanol, and formaldehyde together and added them to the amalgam. The amalgam was not violent, and when stirred, slight bubbles appeared, and the amalgam became thick like dough. I added formaldehyde a second time. Some of it had evaporated while heating the amalgam.

 

[G.Patton]

Your amalgam looks good. Use reflux condenser to avoid a reactant evaporation.

 

[G.Patton]

In addition, I have no Idea why do you add there ethanol on the final stage. In the tutorial, I clearly wrote this:

Meth hydrochloride has mp 170-175*C, it's okay.

 

[wael gano]

Sorry
I read in another synthesis of yours
You evaporate Dcm and add ethanol to the base, then the gas
But okay if the free base of meth in the solvent is Dcm
Adding hydrogen chloride gas is normal, so I can do this

 

[Mo0odi]

Can you explain the reaction mechanism?

What is the difference when we add hydrochloric acid and when we add hcl gas

 

[Mo0odi]

@G.Patton

The whole reaction mass is treated with 20 % HCl to pH 3 and extracted by DCM or petrolium ether 3 x 75 mL. DCM extracts are combined. Resulting water layer from filtration is alkalinized by 20% NaOH aq to pH 12 and extracted with DCM or petrolium ether 3 x 75 mL. Organic layers with methamphetamine (4) are combined (from first and second extraction of alkilized water layer), dried over Na2SO4 or MgSO4 anhydrous and concentrated in vacuum.


Please can you explain this step further

I think @wael gano faced a problem with this step

 

[G.Patton]

What exactly don't you understand? At first - acid extraction, then - base extraction, evaporation of solvent and acidification. I can't write more clearly or simplify this part. It is already simple as possible.

 

[wael gano]

I had no problems with acid-base extraction
All you have to do is add acid and extract with solvent
Then add the alkali, extract again and combine the extracts together

 

[OrgUnikum]

First of all one would have to know what concentration the 3 ml formaldehyde in water solution was. As if there is more formaldehyde then absolutely necessary, more then one molecule formaldehyde for every molecule amphetamine present, then there will be the result a lot of di-methyl amphetamine, say not only one but two formaldehyde molecules (methyl) attaching to the Amphetamine.

Also I am afraid Al/Hg is NOT a very good method for this, it will always give just mediocre results. Catalytic hydrogenation though is known to work very well.