Synthesis of Methamphetamine from P2P and NaBH4 Reduction

GhostChemist

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Reactions proceed according to Scheme 1.
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Scheme 1
Reagents and Materials:
  • 10 g of pure P2P (steam distillation purified)
  • 45-55 g of silica gel d=2.5-4 mm (NOT powder)
  • 3 g of sodium borohydride (equivalent in moles)
  • 65 ml of absolute isopropyl alcohol
  • 18.1 – 20 ml of 35-40% aqueous methylamine
  • 50-100 g of anhydrous sodium sulfate Na2SO4
  • 200-250 ml of dichloromethane
  • 50-100 g of ammonium chloride NH4Cl
  • 50 ml of concentrated sulfuric acid (88%)
  • 10-15 ml of diethyl ether
  • 200-300 ml of distilled water
  • 5-10 g of sodium hydroxide
  • 500-1000 g of ice
  • cool packs
  • 1 L three-neck flask
  • Distillation setup
  • Vacuum filtration setup
  • Chemical beakers
  • Glass adapters
  • 2 L separating funnel
  • Heater
Download Video

Synthesis

Stage 1

Prepare the mixture in the container one day before the synthesis by combining 20 ml of methylamine, 65 ml of absolute isopropyl alcohol, and 15 g of anhydrous sodium sulfate. Add 2-5 g of silica gel to the mixture and periodically stir the mixture with vigorous shaking. Fig 1
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Fig 1

Add 40 g of silica gel into a three-necked flask, connect the absorbers (a calcium chloride tube with silica gel and hygroscopic cotton), and let it stand for 0.5-1 hour for drying. Fig 2
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Fig 2

Pour the pre-prepared and dried methylamine solution in alcohol into the reactor, additionally rinsing the sodium sulfate with portions of isopropyl alcohol. In the case where P2P was not pre-dried, set up a separating funnel with a layer of silica gel and introduce P2P into the reactor in portions. After adding all of P2P, rinse the remaining residue with several portions of isopropyl alcohol. Stir the resulting reaction mass for 2 hours, during which the temperature increases from 22 to 30°C, which should be considered for larger synthesis volumes. Fig 3
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Fig 3

The next step is to cool the reaction mixture (RM) to 0-5°C. Fig 4
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Fig 4

Sodium borohydride is added to the reaction mixture (RM) in small portions to prevent the temperature from rising above +15°C (for about 3 hours). After adding all the sodium borohydride, the RM is stirred for 1-1.5 days at a temperature not exceeding +20°C. The temperature is maintained using cold accumulators. Fig 5
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Fig 5

Reaction mass after the reaction. Fig 6
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Fig 6
Stage 2

The reaction mass (RM) in a three-necked flask is filled with water to dissolve the precipitate, then transferred to a separating funnel, and a sodium hydroxide solution is added. The reaction mass should have an appropriate pleasant odor, sometimes with a trace of unreacted methylamine.
Water added to RM. Fig 7
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Fig 7

The silica gel is washed with additional portions of water to extract all of the RM. Then, extraction is performed by adding dichloromethane (DCM). The process is repeated by adding DCM and water for better separation. Fig 8
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Fig 8

The DCM layer is drained into a 1-liter beaker, and anhydrous sodium sulfate is added. Fig 9
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Fig 9

Dried extract of methamphetamine in DCM. Fig 10
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Fig 10
Stage 3

The dried extract in DCM is introduced into a 500 ml flask (the drying agent is washed with additional portions of DCM!). Fig 11
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Fig 11

The distillation setup is assembled. DCM is distilled off at the temperature 90-100°C. Complete distillation of DCM is not important. Fig 12
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Fig 12

The oil after DCM distilled off, should have a pleasant amine-like odor, significantly different from the smell of methylamine. Fig 13
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Fig 13

Stage 4

The oil obtained in Stage 3 is transferred to a beaker, and an additional 10-20 ml of ethanol is rinsed from the distillation flask. Fig 14
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Fig 14

A hydrogen chloride generator is assembled. Fig 15
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Fig 15

The methamphetamine free base should have an alkaline reaction until it is saturated with hydrogen chloride. Fig 16
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Fig 16

After the beginning of hydrogen chloride evolution from the tube, you can gradually immerse it in the solution to prevent it from getting sucked in! After full saturation, the solution should have a pink, raspberry, or dark red color depending on the purity of the reagents used during the synthesis. Fig 17
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Fig 17

Next, the obtained solution is evaporated until crystallization occurs. Fig 18
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Fig 18

Fully crystallized reaction mass. Fig 19
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Fig 19

The crystallized methamphetamine hydrochloride is mixed with diethyl ether and thoroughly stirred into a paste-like mass. The resulting paste is transferred onto a vacuum filter. Fig 20
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Fig 20

The methamphetamine hydrochloride is filtered, if necessary, washed with additional portions of ether (ethylacetate or Et2O) (in case of heavy contamination, acetone is also added). Fig 21
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Fig 21

The obtained methamphetamine hydrochloride. Fig 22
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Fig 22


The product yield is 60 - 79 %



Recommendations:
  • All reagents and glassware must be dry.
  • A small portion of silica gel can be added to sodium borohydride.
  • The size of the silica gel is 2.5-4 mm.
  • Do not use silica gel in powder form.
 
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Mo0odi

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thank you for your effort
 

jasper

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The most awaited synthesis in my life
 

hunter12

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Can this synthesis be done in larger scale, like 1-2 kilo
 

Throw-off

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Throw-off

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Is the sodium sulfate just used as a drying agent for the DCM? Is there a reason to use Sodium sulfate over magnesium sulfate?
 

GhostChemist

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Is the sodium sulfate just used as a drying agent for the DCM? Is there a reason to use Sodium sulfate over magnesium sulfate?
Throw-offno, you can use any drying agent as sodium sulfate or magnesium sulfate. but don`t use MgClO4 as drying agent
 

jotoy

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How to use methylamine hcl in this process?
 

GhostChemist

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Throw-off

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You cant just disolve methylamine into alchohol to make a solution
jotoyAre you dyslexic? When did I state methylamine HCl could be dissolved in alcohol? Freebase the hcl and it releases the gas and makes water and salt as bi-product.. I swear some of you retards shouldn't be messing with chemicals.
 

hunter12

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Can we please have the secret to big nice shards of meth crystals. Tried almost all the recrystalization on the forum but non of them give big crystals.
 

lalalander

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Can we please have the secret to big nice shards of meth crystals. Tried almost all the recrystalization on the forum but non of them give big crystals.
hunter12You need to separate the isomers. The D and L isomers form large rocks on their own, but not together.
 
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hunter12

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You need to separate the isomers. The D and L isomers form large rocks on their own, but not together.
lalalanderThank you so much. After separation what method you use to make transparent glass from the different insomers
 

hacke8

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Hi, gentlemen, you need to dry the reagent before production, but you need to use 40% methylamine aqueous solution, which contains water. What's the use of drying like this?
 

Asan1973

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The reaction mass (RM) in a three-necked flask is filled with water to dissolve the precipitate, then transferred to a separating funnel, and a sodium hydroxide solution is added. The reaction mass should have an appropriate pleasant odor, sometimes with a trace of unreacted methylamine.
Water added to RM


Distinguished experts, I would like to know how much sodium hydroxide solution is added here? What is the ratio of sodium hydroxide to water. Do I need to add sodium hydroxide solution if I extract with DCM like in the video?
 

GhostChemist

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The reaction mass (RM) in a three-necked flask is filled with water to dissolve the precipitate, then transferred to a separating funnel, and a sodium hydroxide solution is added. The reaction mass should have an appropriate pleasant odor, sometimes with a trace of unreacted methylamine.
Water added to RM


Distinguished experts, I would like to know how much sodium hydroxide solution is added here? What is the ratio of sodium hydroxide to water. Do I need to add sodium hydroxide solution if I extract with DCM like in the video?
Asan1973Water layer must be with alkali pH
ratio of sodium hydroxide to water not important, for example use 10 g NaOH in 50-100 ml of water
 
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