Methamphetamine synthesis from P2P via Aluminum amalgam

WillD

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Equipment and glassware:

Reagents:
  • Ethanol 200 ml;
  • Aqueous methylamine (free base) 200 ml 25%;
  • Cut aluminum foil 40 g;
  • Mercury chloride (HgCl2) 0.30 g or mercury 2 nitrate (Hg(NO3)2) 0.359 g;
  • Distilled water;
  • Potassium hydroxide 120 g;
  • Diethyl ether (or petroleum ether) 750 ml;
  • Magnesium sulphate anhydrous (MgSO4) ~30 g;
  • Acetone ~150 mL;
  • Concentrated hydrochloric acid (HCl 36%) ~12 mL;
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Synthesis:
1. Phenyl-2-propanone 40 g, ethanol 200 ml, aqueous methylamine (free base) 200 ml 25%, cut aluminum foil 40 g and mercury chloride 0.30 g (or mercury 2 nitrate 0.359 g) are placed into a 5 L round bottom flask.
2. A reflux condenser is installed and reaction mixture is refluxed for 2 hours and cooled down to a room temperature.
3. The reaction mixture is poured into a ice-water (1:1 v/v) beaker through a sieve filter (to get rid of solid Al/Hg), flask has to be washed off from residues of reaction mixture to a beaker. The reaction mixture in the beaker is alkalized with potassium hydroxide aq solution (120 g KOH in 250 ml H2O).
4. Then, the solution is extracted with
diethyl ether (or petroleum ether) 750 ml.
5. Ether extract with methamphetamine free base is
dried over MgSO4. After that, a solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum.
6. Next, crude methamphetamine free base is
distilled with vacuum to give pure 1-phenyl-2-methylaminopropane (methamphetamine) with 70% yield.
7. Methamphetamine free base is dissolved in x3 volume of dry acetone.
8. Concentrated hydrochloric acid (HCl 36%) is added dropwise to reach
pH 6.
9. The mixture is put into a freezer for 12 hours, methamphetamine is crystalized there.
10. Methamphetamine crystals are
vacuum filtered, washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber).

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Toomuchname

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What do you mean by "Poured into ice-water"?
We pour the refluxed mixture into ice-water?

And if yes, how much water do I have to use?
 

Mclssmxxl

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If I were to guess it’s for the CRAP(Crude reagent and product) to have a place to go to that’s not your organic layer.
 

Toomuchname

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You’re probably right, thanks🤪
 

G.Patton

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Yes. The volume of water is 1:1.
 

medosal

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Can we replace Koh by Naoh ?
 

G.Patton

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Hello, yes
You have to get methylamine free base. Hydrochloric salt will not work.
 

bndr

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Methylamine freebase is a gas, in this procedure he uses methylamine HCL, the sodium hydroxide freebases it as its added to the reaction. So yes Methylamine HCL can be used. Its all ive ever used....
 

WilliamK

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We are not using pure methylamine but 25% solution which is dissolved in water.
In this form, it's obliviously a liquid
 

Mr.Blanks00

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sorry to ask what is another name for aluminum turning, can aluminum foil be used.
 

G.Patton

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johnny.b

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This reaction work when You use methylamine 33% in methanol?
 

G.Patton

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I think yes.
 

ASheSChem

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it can be replace by isopropanol?
 

primitiveintelectual

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I don't understand step 5 to 6

step 5. When evaporate diethyl ether, We will get freebase.
what does it mean freebase?
It means a powder methamphetamine?
How then in Step 6 I have to distilled this powder methamphetamine?
Should I dissolve the methamphetamine powder in the water (1:1) and distilled?
Why is step 6 needed? Could I skip step 6?
When in step 5 evaporated diethylether, I got a powder methamphetamine, Can I go straight to step7?

Sorry my stupid questions.
 

G.Patton

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Methamphetamine base is also named amphetamine freebase or just free base. Amphetamine is organic base by presence of -NH2 group.
Methamphetamine powder is methamphetamine salt, which is obtained after step 8
Methamphetamine free base is liquid and distilled with vacuum
no
Yes but your Methamphetamine salt product will have a low quality.
you'll get methamphetamine free base
 

Fenster

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Can Methanol replace ethanol as solvent?
 
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