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William D.

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ZeA8S2fMdw

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;
Download Video

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).

Related topic
 
Last edited by a moderator:

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?
 

Dafunkphenomena

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View attachment 1396

is that synth way scalable? x10 x 20 etc?

tnx in advance!


Synthesis:
1. Mixed of 40 g phenyl-2-propanone, 200 ml ethanol, 200 ml 25% aqueous methylamine, 40 g aluminum turnings and 0,30 g mercuric chloride.
2. Refluxed 2 hours.
3. Poured into ice-water, alkalinized with 120 g. potassium hydroxide.
4. Extracted with 750 ml diethyl ether.
5. Extract dried and evaporated.
6. The residue was distilled in vacuum to give 1-phenyl-2-methylaminopropane, 70% yield.
7. Dissolved in 3 amounts of dry acetone.
8. Dropwise conc. HCl acid at pH - 6.
9. Put in freezer for 12 hours.
10. Filtered and dry.
William Dampier
 

medosal

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Reaction scheme:
View attachment 1396


Synthesis:
1. Mixed of 40 g phenyl-2-propanone, 200 ml ethanol, 200 ml 25% aqueous methylamine, 40 g aluminum turnings and 0,30 g mercuric chloride.
2. Refluxed 2 hours.
3. Poured into ice-water, alkalinized with 120 g. potassium hydroxide.
4. Extracted with 750 ml diethyl ether.
5. Extract dried and evaporated.
6. The residue was distilled in vacuum to give 1-phenyl-2-methylaminopropane, 70% yield.
7. Dissolved in 3 amounts of dry acetone.
8. Dropwise conc. HCl acid at pH - 6.
9. Put in freezer for 12 hours.
10. Filtered and dry.
William DampierCan we replace Koh by Naoh ?
 

medosal

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Reaction scheme:
View attachment 1396


Synthesis:
1. Mixed of 40 g phenyl-2-propanone, 200 ml ethanol, 200 ml 25% aqueous methylamine, 40 g aluminum turnings and 0,30 g mercuric chloride.
2. Refluxed 2 hours.
3. Poured into ice-water, alkalinized with 120 g. potassium hydroxide.
4. Extracted with 750 ml diethyl ether.
5. Extract dried and evaporated.
6. The residue was distilled in vacuum to give 1-phenyl-2-methylaminopropane, 70% yield.
7. Dissolved in 3 amounts of dry acetone.
8. Dropwise conc. HCl acid at pH - 6.
9. Put in freezer for 12 hours.
10. Filtered and dry.
William Dampiercan i use methylamine HCL instead methylamine
 

G.Patton

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bndr

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Hello, yes

You have to get methylamine free base. Hydrochloric salt will not work.
G.PattonMethylamine 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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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....
bndrWe 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.
 

johnny.b

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

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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what does it mean freebase?
primitiveintelectualMethamphetamine base is also named amphetamine freebase or just free base. Amphetamine is organic base by presence of -NH2 group.
It means a powder methamphetamine?
Methamphetamine powder is methamphetamine salt, which is obtained after step 8
How then in Step 6 I have to distilled this powder methamphetamine?
Methamphetamine free base is liquid and distilled with vacuum
Should I dissolve the methamphetamine powder in the water (1:1) and distilled?
no
Why is step 6 needed? Could I skip step 6?
Yes but your Methamphetamine salt product will have a low quality.
When in step 5 evaporated diethylether, I got a powder methamphetamine
you'll get methamphetamine free base
 

Fenster

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Can Methanol replace ethanol as solvent?
 
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