Methamphetamine via Al/Hg synthesis report

GhostChemist

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The reactions proceed according to Scheme 1.
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Reagents and materials:

  • Aluminum foil, 14 µm, 10.5 g
  • Mercury(II) chloride, 0.1 g
  • Distilled water, 3 L
  • P2P (phenyl-2-propanone), 10 g
  • Methylamine 39%, 25-30 mL
  • Sodium chloride, 10 g in 30 mL water
  • Isopropylalcohol (IPA), 150 mL
  • Dichloromethane, 150-200 mL
  • Ethanol 88%, 25 mL
  • Ammonium chloride, 50-100 g
  • Concentrated sulfuric acid 80%, 15 mL
  • Technical-grade water, 2 L with 500 g of ice
  • Anhydrous sodium sulfate, 20-30 g
  • 10 mL 25% NaOH (sodium hydroxide)
  • Diethyl ether, 15 mL
  • Acetone, 20-25 mL
  • 2 L flask, 500 mL flask, 250 mL flask
  • Three-necked flask, 500 mL, for hydrogen chloride generation
  • Distillation setup
  • Reflux condenser
  • Vacuum filtration setup
  • Separatory funnel
  • Silicone grease
  • Filter paper
  • Funnel
  • Beakers
  • Heater

Stage 1. Preparation of Aluminum Amalgam

Aluminum foil is placed into a 2 L flask and filled with water, ensuring that the foil is submerged beneath the water layer. Fig 1
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Dry mercury(II) chloride is added, and vigorous stirring is performed until hydrogen is actively evolved and a dull appearance appears on the foil. Fig 2
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Fig 3
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Fig 4
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Next, the solution is drained, and the aluminum amalgam is washed twice with distilled water. Fig 5
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Stage 2. Reduction and Extraction

Ice-cold water should be prepared in advance for cooling the flask. To the obtained aluminum amalgam, methylamine, sodium chloride solution, P2P, and IPA are added. The reflux condenser is connected to the flask, and an exothermic reaction begins after approximately 20-30 minutes. Fig 6
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Fig 7
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Fig 8
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The reactor should be cooled if the temperature exceeds 50-60°C. Fig 9
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Fig 10
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Fig 11
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The reaction proceeds completely in approximately 3 hours, during which the reagents transform into a gray mass. Fig 12
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To the reaction mass, 10 mL of 25% NaOH is added to dissolve any unreacted aluminum. The mixture is then allowed to stand for 30-40 minutes until the evolution of hydrogen ceases. Fig 13

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Fig 14
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The solution is separated from the precipitate through filtration, decantation, or centrifugation. The precipitate is further washed with ethanol or IPA to extract the Methamphetamine. Fig 15
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Fig 16
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The obtained Methamphetamine solution is extracted with several portions of dichloromethane. Fig 17
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Fig 18
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The dichloromethane layer is separated using a separatory funnel. If there is an excess of other solvents such as ethanol and isopropanol, there may be a significant increase in volume. In such cases, the organic layer is washed with water to remove the alcohols. Sometimes, it can be challenging to determine the location of the organic (target) layer and the aqueous layer due to their different densities. To determine the location of the target layer, a drop of the solution can be taken with a pipette and rubbed between the fingers. The organic layer (DCM) will almost instantly dry, leaving a pleasant odor of the formed amine, which is distinct from the strong smell of methylamine. The aqueous layer will have a strong alkaline reaction and give a soapy feeling between the fingers when rubbed. The separated DCM layer, if necessary, is filtered and further dried with anhydrous sodium sulfate. Fig 19
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Layer of Methamphetamine extract in dichloromethane after drying with anhydrous sodium sulfate. Fig 20

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Stage 3. Extraction of the Methamphetamine free base and obtaining its hydrochloride.

The dried dichloromethane layer is transferred to a setup for distillation using a water bath. At a temperature of 90°C, the entire dichloromethane is evaporated and distilled off. Fig 21
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Fig 22
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After the distillation process, the flask contains the Methamphetamine free base with its characteristic odor. Fig 23

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The obtained free base Methamphetamine is filtered through a paper filter, and the filter is additionally rinsed with ethanol. Fig 24
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Next, a stream of gaseous hydrogen chloride is passed into the solution of the Methamphetamine in ethanol. Hydrogen chloride gas can be generated by slowly dripping sulfuric acid onto ammonium chloride. Fig 25
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Fig 26
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Fig 27
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During this process, the color of the solution should change from yellow to a rich pink, which is indicative of the formation of the desired Methamphetamine. Fig 28
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Fig 29
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Fig 30
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Fig 31
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Fig 32
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Fig 33
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The obtained solution is evaporated until crystallization occurs. Fig 34
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Fig 35
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Fig 36
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Fig 37
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The crystallized mass is placed on a filter and washed with several minimal possible portions of diethyl ether. Fig 38
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Fig 39
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Fig 40
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Next, the mass is quickly washed with acetone, filtered, and dried on the filter. Fig 41
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Fig 42

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From 10 g of P2P, it should yield 13.84 g of Methamphetamine hydrochloride, which corresponds to a 100% yield, assuming complete conversion and maximum product formation.

The yield in this experiment is as follows:

10.2 g or 73% after washing with diethyl ether

9.6 g or 69% after washing with acetone.


Fig 43
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Mo0odi

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good job
Keep making achievements
 

wael gano

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Welcome
Why did you not use a rotary evaporator for free base distillation?
Wasn't this temperature hurting the free base and making it oxidize? We are used to that the BB forum is keen on this issue. Is everything okay
 

GhostChemist

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Welcome
Why did you not use a rotary evaporator for free base distillation?
Wasn't this temperature hurting the free base and making it oxidize? We are used to that the BB forum is keen on this issue. Is everything okay
wael ganoHi! Yes, hight temperature and air exposure lead to the oxidation of free amine base. Based on experience and observations, the Methamphetamine free base is more stable than the amphetamine free base.
 

wael gano

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Picture of the free base. Nice oil. Looks fine
We thank you for this effort
 

Ortist

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Brother.
During this process, the color of the solution should change from yellow to a rich pink, which is indicative of the formation of the desired Methamphetamine.
GhostChemist
Rich pink means too much acid.

Starting from this point your workup is wrong. Thats why you got 100% yeld which is simply not possible with this reaction. You got too much impurities + mercury salts in your product along with methylamine hydrochloride possible.


Once you got your pink solution, check pH. It must be around 3..5.

Then concentrate your solution.

Then wash it with DCM and all colors will go away.

Then basify with NaOH

Then extract with DCM

Distill DCM off

Carefully acidify to pH 4..6

Evaporate
 

GhostChemist

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Brother.


Rich pink means too much acid.

Starting from this point your workup is wrong. Thats why you got 100% yeld which is simply not possible with this reaction. You got too much impurities + mercury salts in your product along with methylamine hydrochloride possible.


Once you got your pink solution, check pH. It must be around 3..5.

Then concentrate your solution.

Then wash it with DCM and all colors will go away.

Then basify with NaOH

Then extract with DCM

Distill DCM off

Carefully acidify to pH 4..6

Evaporate
OrtistHello!
A 100% yield is not possible.
The theoretical yield is provided for calculating the practical yield as reference information.
The yield for this process is given below.
Secondly, mercury salts cannot form pink compounds, even complex ones, and the content of mercury ions after an alkaline environment will not exceed 0.00026 mol/L.
Excess methylamine, considering the alkaline environment, evaporates during filtration and also transitions into the aqueous phase as it forms an azeotropic mixture with water.
 

gmo

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Can this process be done with precision and principled considerations on a kilo scale?
 

GhostChemist

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Can this process be done with precision and principled considerations on a kilo scale?
gmoHi! In principle, it is possible to carry out the process on 1kg, but it is necessary to consider significant heat generation, so an efficient cooling system is required in the reactor.
 

gmo

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Thank you very much,Wishing you success💎🖐🏻Please make a report on the synthesis of p2p from butanone and benzaldehyde
 

Lordoftheshard 2

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Once you had your freebase you should of disolvedl in 2 to 1 mix of acetone /,free base then tritated with hcl acid to pH 5.5 to 5.8 the evaporated to give you your product also half if that is garbage lmeth so you have to do a resolution with tartaric acid to get the dmeth
 

ossi

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Sodium chloride, 10 g in 30 mL water
GhostChemisti read sodium chloride first time for this synthesis.
i have read this synthesis from several sources and you are the only one using it.
what is the benefit?
 

Mo0odi

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i read sodium chloride first time for this synthesis.
i have read this synthesis from several sources and you are the only one using it.
what is the benefit?
ossiYes, I also did not understand

Please explain
Thank you
 
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