Reaction scheme:Equipment and glassware:
- Retort stand and clamp for securing apparatus (optional);
- Reflux condenser;
- Funnel;
- Sieve filter (kitchen grade is ok);
- Syringe or Pasteur pipette;
- pH indicator papers;
- Beakers (500 mL x2, 250 mL x2, 100 mL x2);
- Vacuum source;
- Vacuum distillation apparatus;
- Laboratory scale (0.01-100 g is suitable);
- Measuring cylinders 250 mL, 100 mL and 20 mL;
- Cold water bath;
- Glass rod and spatula;
- Separatory funnel 1 L (optional);
- Buchner flask and funnel;
- Filter paper;
- Freezer;
Reagents:
Methamphetamine hydrochloride synthesis via Al/Hg
Methamphetamine hydrochloride synthesis via Al/Hg reductive amination with salt formation...
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
Methamphetamine synthesis from P2P via Aluminum amalgam
- Thread starter WillD
- Start date
Performed the procedure twice, first time did not work (I believe from failed aluminum amalgam)
2nd procedure used the following procedure:
1. 10 gr foil, cut to 3x3 cm was amalgamated in solution of 200 mg mercuric chloride in 400 ml warm water until solution became greish and bubbles formed at surface.
2. Water was decanted and aluminum amalgam washed twice with 250 ml cold water
3. To the aluminum amalgam, the following were added quickly: 43 ml methylamine aqueous 40%, 100 ml IPA, 13.4 ml P2P, then another 100 ml IPA.
4. The aluminum pieces were poked with a rod so they stay below the surface of the liquid. Bubbles formed quickly and temperature rose. Flask was immersed in cold water bath when temp reaches over 50C
5. At the 2 hour mark, most of the aluminum was consumed, and 20 ml 25% sodium hydroxide solution was added with stirring, making sure temp does not exceed 50C, then after 3 hours, another 20 ml 25% sodium hydroxide solution was added (5 gr sodium hydroxide in 20 ml water)
6. Reaction was stirred overnight, room temp, then allowed to settle
7. The clear layer was decanted and saved, then 100 ml IPA was added to the grey sludge then stirred for another hour then decanted the IPA layer after particles settled. The aluminum sludge was then vacuum filtered and washed with 2x 50 ml methanol, then all decantations and filtrate were saved
8. Wash with 75 ml brine (25% sodium chloride solution in water) then dry with sodium sulfate with magnetic stirring for 15 mins, then filter
9. Heat the solution to 110C to remove all solvents
10. to the freebase meth, add 150 ml ethanol then add HCl in IPA solution until ph 6
11. Filter the crystals
We acquired crystals from the procedure, a bit bitter, salty crystals.
The melting point of the crystal is very high, it wouldn't roll down the foil after heating, although insufflation and oral both are highly psychoactive with good feedback.
Will be doing A/B extraction on the crystals to see if we can cut out whatever is making it have high melting point
White crystals that were filtered and dried:
After single solvent recrystallization:
anyone have thoughts on what caused the crystal to have high melting point?
2nd procedure used the following procedure:
1. 10 gr foil, cut to 3x3 cm was amalgamated in solution of 200 mg mercuric chloride in 400 ml warm water until solution became greish and bubbles formed at surface.
2. Water was decanted and aluminum amalgam washed twice with 250 ml cold water
3. To the aluminum amalgam, the following were added quickly: 43 ml methylamine aqueous 40%, 100 ml IPA, 13.4 ml P2P, then another 100 ml IPA.
4. The aluminum pieces were poked with a rod so they stay below the surface of the liquid. Bubbles formed quickly and temperature rose. Flask was immersed in cold water bath when temp reaches over 50C
5. At the 2 hour mark, most of the aluminum was consumed, and 20 ml 25% sodium hydroxide solution was added with stirring, making sure temp does not exceed 50C, then after 3 hours, another 20 ml 25% sodium hydroxide solution was added (5 gr sodium hydroxide in 20 ml water)
6. Reaction was stirred overnight, room temp, then allowed to settle
7. The clear layer was decanted and saved, then 100 ml IPA was added to the grey sludge then stirred for another hour then decanted the IPA layer after particles settled. The aluminum sludge was then vacuum filtered and washed with 2x 50 ml methanol, then all decantations and filtrate were saved
8. Wash with 75 ml brine (25% sodium chloride solution in water) then dry with sodium sulfate with magnetic stirring for 15 mins, then filter
9. Heat the solution to 110C to remove all solvents
10. to the freebase meth, add 150 ml ethanol then add HCl in IPA solution until ph 6
11. Filter the crystals
We acquired crystals from the procedure, a bit bitter, salty crystals.
The melting point of the crystal is very high, it wouldn't roll down the foil after heating, although insufflation and oral both are highly psychoactive with good feedback.
Will be doing A/B extraction on the crystals to see if we can cut out whatever is making it have high melting point
White crystals that were filtered and dried:
After single solvent recrystallization:
anyone have thoughts on what caused the crystal to have high melting point?
- By OrgUnikum
rothschild33Guys, you have such nice expensive equipment why the bloody fuck don't you get yourself decent Al-granules but use fucking foil? My Al/Hgs never worked well until I started using granules but then like a charm! The stuff is cheap and unwatched. Do not use foil. If you really want try it later with foil but if you have a good stirrer like you have - foil makes zero sense but fucking up everything. If you have no good stirrer well, thats an excuse but no, better not. Its not just me telling this, look over the old boards in the end everybody tells you to use "Good Al" and this means NOT FOIL.
↑View previous replies…
- By rothschild33
OrgUnikumdefinitely will be going with aluminum turnings going forward, confirmed the foil with aluminum methoxide test.
- By OrgUnikum
hobokingSure. As longs its high purity, say 99.999... or better. My granules are between 0,5 and 2 mm and 99.99999 % Al. Also if spherical or coarse does not really matter, coarse needs a little less time for the higher surface area. Or Al-shavings, whats more or less just what you get when drilling holes into metal, the refuse I mean.
OrgUnikumUsing thicker foil on 10L plus batches, especially on a pressure vessle works perfect.
1 bar 10 temp higher, suggest nitro instead of methylamine but be sure to wash it out with saturated NaCL and baking soda, if lye is added to meta/nitro solvent saves you distilation if using hexane.
1 bar 10 temp higher, suggest nitro instead of methylamine but be sure to wash it out with saturated NaCL and baking soda, if lye is added to meta/nitro solvent saves you distilation if using hexane.
Al/Hg workup can be nasty. Why is everybody decanting, filtering or extracting the sludge?
You can filter through celite in your buchner funnel. this prevents clogging your filter.
But for me the best is, after reaction is completed, adding water and NaOH to basify and then steam distill your product.
No need to deal with the sludge. Just get rid of it after steam distillation and work with a nice clear solution.
Be careful, sometimes some beads of metallic mercury comes along with your steam distillate. Get rid of it aswell.
Al/Hg isn't that bad when you get used to it.
You can filter through celite in your buchner funnel. this prevents clogging your filter.
But for me the best is, after reaction is completed, adding water and NaOH to basify and then steam distill your product.
No need to deal with the sludge. Just get rid of it after steam distillation and work with a nice clear solution.
Be careful, sometimes some beads of metallic mercury comes along with your steam distillate. Get rid of it aswell.
Al/Hg isn't that bad when you get used to it.
What can replace Mercury chloride
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