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Methamphetamine Synthesis From P2P Via Al/Hg

GhostChemist

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The reactions proceed according to the Scheme 1.
EKJWDbouiX

Reagents and Materials:

  • Aluminum foil 14 µm, 6 g
  • Mercury(II) chloride, 0.05 g
  • Distilled water, 2-3 liters
  • P2P (from p2np via NaBH4 reduction and steam distill) 5 g
  • Aqueous methylamine 39%, 15 ml
  • Sodium chloride, 5 g in 15 ml water
  • IPA (isopropyl alcohol) or ethanol, 100 ml
  • DCM (dichloromethane) 75-100 ml
  • Ammonium chloride, 50-100 g
  • Concentrated sulfuric acid 80%, 20-25 ml
  • Technical-grade water, 2 liters with 500 g of ice
  • Anhydrous sodium sulfate, 20-30 g
  • 5 ml 25% NaOH
  • Diethyl ether, 5-10 ml
  • 2-liter, 500 ml, 250 ml flasks
  • 500 ml three-necked flask for generating hydrogen chloride
  • Reflux condenser
  • Setup for solvent distillation with a water bath
  • Vacuum filtration setup
  • Separatory funnel
  • Silicone grease for grinding
  • Filter paper
  • Funnels
  • Beakers
  • Heater

Synthesis Procedure

A 2-liter flask is charged with aluminum foil and filled with water so that the foil is submerged beneath its layer. Dry mercury(II) chloride is added, and the mixture is vigorously stirred until active hydrogen evolution occurs and a dull appearance forms on the foil. Fig 1
KU6T2oD1bh

Active hydrogen evolution during the preparation of an amalgam. Fig 2
Vr0LRnmGak

Methylamine, sodium chloride solution, p2p and ethanol are added to the prepared amalgam. A reflux condenser is connected. Fig 3
17J6QfVUc0

When the flask is strongly heated (above 40-50°C), cooling in an ice bath is necessary. Fig 4
SdMnISYpkb

Appearance of the reaction mixture inside the flask during the active progression of the process. Fig 5
ZxtcnWSIEb

Next, a sodium hydroxide solution is added to the reaction mixture to dissolve excess aluminum, and it is left for approximately 1 hour. The resulting reaction mixture is poured onto a filter without further washing of the sludge. Fig 6
LWmVv4QDot

The obtained amine solution is extracted with several portions of DCM (dichloromethane). Fig 7
8uPirKdOox

The DCM layer is separated in a separating funnel. The separated DCM layer, if necessary, is filtered, dried with anhydrous sodium sulfate, and distilled to an oil at T=90°C.
The extract in DCM is distilled before distillation. Fig 8

MHguFt1VhT

Free base after distillation of DCM. Fig 9
BtORgicNqP

Next, a stream of gaseous hydrogen chloride is passed into the solution of the amine in ethanol until a strong acidic reaction and the appearance of a pink color in the solution. The obtained solution is evaporated to crystallization. Hydrogen chloride is obtained by adding sulfuric acid to ammonium chloride.
Crystallization of the amine hydrochloride. Fig 10

JFRghbCINJ

The crystallized amine hydrochloride. Fig 11
Zw9CsiNc0m

The crystallized mass is washed with diethyl ether (5-10 ml), filtered, and dried. Fig 12
UcGE2dgIpy

The yield without additional sludge washing was 4.5 g, or 65% of the theoretical yield.
The loss in the sludge is 0.5 g, or 7.2%.
 
Last edited by a moderator:

Djdrama

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I don't get you well. You use 5 gram of p2p and got 72.2% which is 4.5 grams?
 

The Alchemist

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I don't get you well. You use 5 gram of p2p and got 72.2% which is 4.5 grams?
DjdramaSays loss of 0.5 in sludge so isn't that 4g so 80% before recrystallization?
 

The Alchemist

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Nice write up! Is there a final recrystallization phase you'd recommend?
 

Jordan Belfort

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Why no-where bubbeling occurs in hexane? And washing with hot water with NaCl and baking soda take alot of impurities.

Nevertheless if you use methanol instead of IPA you can do a direct extraction from the reaction mixture after adding lye with hexane.
 

Jordan Belfort

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Why no-where bubbeling occurs in hexane? And washing with hot water with NaCl and baking soda take alot of impurities.

Nevertheless if you use methanol instead of IPA you can do a direct extraction from the reaction mixture after adding lye with hexane.
Jordan BelfortAlso if you use nitromethane instead of methylamine you don't need to do coolin, plus you can distill and reuse your methylamine source. Less waste and less coste
 
View previous replies…

CryoThio

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Also if you use nitromethane instead of methylamine you don't need to do coolin, plus you can distill and reuse your methylamine source. Less waste and less coste
Jordan BelfortWait, I'm pretty sure I've read that using nitromethane runs hotter than using methylamine, because it is doing two reductions are once. I've never seen that it should run cooler.
 

Jordan Belfort

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Wait, I'm pretty sure I've read that using nitromethane runs hotter than using methylamine, because it is doing two reductions are once. I've never seen that it should run cooler.
CryoThioYou need cooling because of the boiling temprature of methanol, you boil of the methylamine. With nitromethane you don't, also nitromethane works as a suitable solvent.

Nitromethane also creates a aezotrope with methanol increasing its boiling point to 80 degrees
 

CryoThio

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You need cooling because of the boiling temprature of methanol, you boil of the methylamine. With nitromethane you don't, also nitromethane works as a suitable solvent.

Nitromethane also creates a aezotrope with methanol increasing its boiling point to 80 degrees
Jordan BelfortAh OK, I understand what you are saying now.

That is good information.

I also think I read that the nitromethane route is less "dense" in that one can run larger reactions with the same exotherm. If that makes sense.
 

Jordan Belfort

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Is this amalgam synth with nitromethane as a solvent and donor of methylamine?
GhostChemistNo, it's a modified barbier reaction with a form of zinc which then becomes sort of complex and somehow can take a little water. quenching the reaction with water doesn't work anymore.

it's a super grignard reaction, but it's barbier because a single pot.
 

Jordan Belfort

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This picture indicates the reaction of nitromethane reduction with hydrochloric acid and tin metal
To produce methylamine gas
wael ganoyou worked with nitromethane before ? I have problems isolating the product that I will probably acified it in the future with citric acid and then vacuum distill all of, and from there one add lye to basify it again and the further vacuum distill the base (and water then ofcourse) and then extract distiliate with hexane and bubble dry HCL gas through it.

Or just freeze it and recrystallize it with IPA.
 

minnimus

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Also if you use nitromethane instead of methylamine you don't need to do coolin, plus you can distill and reuse your methylamine source. Less waste and less coste
Jordan BelfortCan you please explain how to use nitromethane instead of methlamin
In this reaction?

Is it possible do
Use RC fuel meaning 10% nitromethane 90%methonol and mix it with the rest of the recipe?
 

Marocamora

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The reactions proceed according to the Scheme 1.

Reagents and Materials:

  • Aluminum foil 14 µm, 6 g
  • Mercury(II) chloride, 0.05 g
  • Distilled water, 2-3 liters
  • P2P (from p2np via NaBH4 reduction and steam distill) 5 g
  • Aqueous methylamine 39%, 15 ml
  • Sodium chloride, 5 g in 15 ml water
  • IPA (isopropyl alcohol) or ethanol, 100 ml
  • DCM (dichloromethane) 75-100 ml
  • Ammonium chloride, 50-100 g
  • Concentrated sulfuric acid 80%, 20-25 ml
  • Technical-grade water, 2 liters with 500 g of ice
  • Anhydrous sodium sulfate, 20-30 g
  • 5 ml 25% NaOH
  • Diethyl ether, 5-10 ml
  • 2-liter, 500 ml, 250 ml flasks
  • 500 ml three-necked flask for generating hydrogen chloride
  • Reflux condenser
  • Setup for solvent distillation with a water bath
  • Vacuum filtration setup
  • Separatory funnel
  • Silicone grease for grinding
  • Filter paper
  • Funnels
  • Beakers
  • Heater

Synthesis Procedure

A 2-liter flask is charged with aluminum foil and filled with water so that the foil is submerged beneath its layer. Dry mercury(II) chloride is added, and the mixture is vigorously stirred until active hydrogen evolution occurs and a dull appearance forms on the foil. Fig 1

Active hydrogen evolution during the preparation of an amalgam. Fig 2

Methylamine, sodium chloride solution, p2p and ethanol are added to the prepared amalgam. A reflux condenser is connected. Fig 3

When the flask is strongly heated (above 40-50°C), cooling in an ice bath is necessary. Fig 4

Appearance of the reaction mixture inside the flask during the active progression of the process. Fig 5

Next, a sodium hydroxide solution is added to the reaction mixture to dissolve excess aluminum, and it is left for approximately 1 hour. The resulting reaction mixture is poured onto a filter without further washing of the sludge. Fig 6

The obtained amine solution is extracted with several portions of DCM (dichloromethane). Fig 7

The DCM layer is separated in a separating funnel. The separated DCM layer, if necessary, is filtered, dried with anhydrous sodium sulfate, and distilled to an oil at T=90°C.
The extract in DCM is distilled before distillation. Fig 8


Free base after distillation of DCM. Fig 9

Next, a stream of gaseous hydrogen chloride is passed into the solution of the amine in ethanol until a strong acidic reaction and the appearance of a pink color in the solution. The obtained solution is evaporated to crystallization. Hydrogen chloride is obtained by adding sulfuric acid to ammonium chloride.
Crystallization of the amine hydrochloride. Fig 10


The crystallized amine hydrochloride. Fig 11

The crystallized mass is washed with diethyl ether (5-10 ml), filtered, and dried. Fig 12

The yield without additional sludge washing was 4.5 g, or 65% of the theoretical yield.
The loss in the sludge is 0.5 g, or 7.2%.
GhostChemistGreat job please download this video on this page if you don't mind and thank you
 
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