Ephedrone From Ephedrine Hydrochloride

[G.Patton]

Introduction​

Ephedrine and pseudoephedrine, commonly used in clandestine laboratories in synthetic oxidation with potassium permanganate to form 2-methylamino-1-phenylpropan-1-one. This ketone product of methamphetamine, termed "ephedrone", "methcathinone" and "Jeff". Some people on BB Forum are interested in this synthesis way and I decided to post this tutorial to shed light on this issue.​

Ephedrone (methcathinone) Hydrochloride Salt​

Equipment and glassware:​

• 2000 mL Erlenmeyer flask or flat bottom flask;
• Magnetic stirrer;
• Funnel;
• Laboratory scale (0.1 g-200 g is suitable);
• HCl laboratory generator;
• Rotavap machine with water bath (optional);
• 0.5 L Separatory funnel;
• Column for flash chromatography with tap (optional);
• 0.5 L (x2), 200 ml (x2), and 100 ml (x3) beakers;

Reagents:​

• Methylene chloride (DCM) 350 mL;
• Glacial acetic acid (CH3COOH) 10 mL;
• Distilled water 100 mL;
• Potassium permanganate (KMnO4) 2 g;
• Ephedrine hydrochloride 2 g;
• Sodium hydrogen sulfite (NaHSO3);
• Sodium hydroxide 5N (NaOH, 18.08% aq. sln.);
• Sulfuric acid 0.5N (H2SO4, 2.43% aq snl);
• Sodium bicarbonate (NaHCO3) aq. sln.;
• Alumina powder (optional) ~40 g;
• Hexane ~100 mL;

Difficulty rating: 2/10

Procedures:​

1. A 2000 mL Erlenmeyer flask, equipped with a magnetic stirring bar, was charged with methylene chloride (DCM, 200 mL), glacial acetic acid (CH3COOH, 10 mL), water (100 mL), potassium permanganate (2 g), and ephedrine hydrochloride (2 g).

2. The solution was stirred at room temperature for 30 min.

3. This was followed by the addition of sufficient sodium hydrogen sulfite (NaHSO3) to reduce the precipitated manganese dioxide (MnO2).

4. The aqueous phase was made basic with 5N sodium hydroxide (NaOH, 18.08% aq. sln.), stirred for a few minutes, and the methylene chloride was separated with help of separatory funnel. [this step is base extraction]

5. The organic layer was extracted with 0.5N sulfuric acid (H2SO4, 2.43% aq snl). [this step is acid extraction]

6. Isolation of the acid layer, followed by basification with sodium bicarbonate (NaHCO3) aq. sln. and extraction with methylene chloride (DCM, 50 mL, three times), removed the product into the organic phase (DCM layer).

7. The solvent (DCM) was concentrated by rotary evaporation, followed by column chromatography (this step is optional) through neutral alumina (aluminium oxide Al2O3) with methylene chloride.

8. Solvent removal through rotary evaporation produced a colorless liquid which was dissolved in hexane.

9. Gaseous HCl was bubbled into the hexane to precipitate the amine hydrochloride to produce a 1 g (50%) yield of 2-methylamino-1-phenylpropan-1-one hydrochloride (d,l-Ephedrone (methcathinone) hydrochloride). Enolizable ketone will result in racemic d,l-ephedrone.​

 

[bigbadbear]

it's so nice
In some countries, they sell this instead of meth.and No one will know the difference

 

[HIGGS BOSSON]

Methcathinone has a very short action from methamphetamine, so an experienced user can easily identify the substitution.

 

[tentamtenztamtad]

tell me how to clean it

 

[tinang]

Nice guide! I wrote down all the reactions that I expect to occur.

As for the oxidation:

• HCl from salt will dissociate into H+ and Cl- ions
• 3C10H15NO + 2KMnO4 => 3C10H13NO + 2H2O + 2MnO2 + 2KOH
• KOH will dissociate into K+ and OH- ions

As for removing manganese:

• 2MnO2 + 4NaHSO3 => Mn2 + 4 NaHSO4
• NaOH dissociates into Na+ and OH- ions (generates heat)
• OH- will bind with Mn2 => 2NaOH => Mn(OH)2 + 2Na+ (ions)
• Any Na+ imbalance will form NaOH + H2 (be careful)
• Hydrogen gas will evaporate leaving Na+ and OH- ions
• NaHSO4 + NaOH => Na2SO4 + H2O
• Na2SO4 dissociates into 2Na+ and SO4- ions (again be careful about hydrogen)
• Mn(OH)2 is hardly soluble solid which can be filtered

As for removing acid:

• H2SO4 dissociates into HSO4- and H+ ions
• HSO4- dissociates into SO4²- and H+ ions
• OH- ions are joined by H+ ions to create H2O
• Remaining are H+, Na+, SO4-, SO4²- ions, and Cl- ions in traces
• NaHCO3 is added and with H+, SO4-, Na+ ions produes Na2SO4 + H2O + CO2
• CO2 evaporates, leaving DCM, H2O, CH3COOH, Na2SO4, C10H13NO
• All the liquids can be evaporated (DCM, H2O, CH3COOH)
• Na2SO4 is highly solluble in water but can be filtered as solid in DCM
• Is is used in food coloring and is safe for human consumption in case of any mistake

After removing Na2SO4 and evoporating all liquids we should have only have C10H13NO remaining

Please correct me if anything is wrong, I would like to understand this reaction the best that I can due to Mn used

I also believe this could be done with higher Ephedrine and and KMnO4 proportion to the solvents.
Would like to know G.Patton opinion since this might not be viable for higher quanitities (10g - 3.5L DCM with this ratio).

 

[tinang]

I wrote a bunch of wrong information above because I didn't fully understand the reaction
Here is the correction with some extra details:

• All the starting compounds are in aqueous phase (H2O and CH3COOH)
• Ephedrone will move to the organic layer (DCM) after oxidation
• NaHSO3 will reduce MnO2 to Mn(OH)2 (solid) and leave NaHSO4 (acid)
• NaOH will react with acids leaving CH3COONa and Na2HSO4
• Tip for separation, organic layer (DCM) is on the bottom since it's more dense
• After separating layers there will only be Ephedrone in DCM in any significant amount, the rest is done for safety (for us)
• Our new layers are DCM (organic layer) and NaHSO4 (aqueous phase)
• NaHSO4 creates Ephedrone*HSO4 salt which dissolves in acid and can be separated and new DCM can be added
• NaHCO3 breaks down the HSO4 salt and neutralizes H2SO4 to Na2HSO4 and H2O
• The free base Ephedrone is extracted organic layer since it dissolved better in the organic layer
• There is no hydrogen gas created at any step

Here is a picture with the summary (red targeted compounds, yellow resulting compounds, green added compounds):
]

 

[Donotdon't]

Can you please upload a video for this synthesis?

 

[badboy345]

much more easy get bromopropiophenone like ephedrone

 

[WillD]

This method is interesting for those whose raw material is ephedrine pills.