Easiest way to amphetamine in the kitchen... (I think)
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1. Do some nitroethane
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(from:
https://www.thevespiary.org/rhodium/Rhodium/chemistry/nitroalkane.html
)
Nitroethane from Sodium Ethyl Sulfate [4]
1.5 mole sodium nitrite (103.5g) is intimately mixed with 1 mole of sodium ethyl sulfate (158g) and 0.0625 moles of K2CO3 (8.6g). The mixture is then heated to 125-130°C, at which temperature the nitroethane distills over as soon as it is formed. The heating is discontinued when the distillation flow slackens considerably, and the crude nitroethane is washed with an equal amount of water, dried over CaCl2, and if needed, decolorized with a little activated carbon. The nitromethane is then re-distilled, collecting the fraction between 114-116°C. Yield 46% of theory.
Preparation of Sodium Ethyl Sulfate
Method 1 [1]
To prepare the sodium salt of ethyl hydrogen sulfate, a mixture of alcohol and H2SO4 is boiled under reflux, cooled, and an excess of calcium carbonate is added. The ethyl hydrogen sulfate is converted into the soluble calcium ethyl sulfate, whilst the excess of H2SO4 is removed as insoluble calcium sulfate. The aqueous filtrate is then mixed with just sufficient sodium carbonate to give sodium ethyl sulfate, the insoluble calcium carbonate being now filtered off. The solution of sodium ethyl sulfate can be concentrated on the water-bath without appreciable hydrolysis, and the sulfate finally crystallized out.
Place 40ml (32g) of rectified spirit in a 250ml round-bottomed flask, and slowly add. 16ml (30g) of concentrated sulfuric acid, keeping the liquid in the flask well shaken throughout the addition to ensure thorough mixing. Fit a reflux condenser to the flask, and heat the latter on a gauze so that the mixture boils gently for 45 minutes. Then cool the product and pour it into 200ml of cold water contained in a large (8-inch) evaporating-basin or in a shallow earthenware dish. Now add 23g of finely powdered calcium carbonate with stirring to the acid solution. It is essential to add the calcium carbonate as a fine stream of powder, and to stir the latter immediately into the bulk of the solution: for this purpose, it is best to sift the carbonate through a fine sieve directly into the liquid, or alternatively to add it from a spatula, tapping the latter gently over the liquid to ensure steady addition of the finely powdered chalk. If the carbonate is added carelessly several grams at a time, it becomes rapidly covered with insoluble calcium sulfate, which protects it from further reaction: in these circumstances, at least 10 times the theoretical quantity of the carbonate may be required and the evolution of carbon dioxide may continue for several hours. The addition of the calcium carbonate should take about 30 minutes, and the well-stirred mixture should finally be neutral to litmus-paper. Now heat the mixture on a water-bath, using a thermometer as a stirrer, until the temperature reaches 60°C, and then filter at the pump through a wide Buchner funnel: at this temperature, filtration should be rapid. Finally wash the residue of calcium sulfate on the filter with a small quantity of hot water, adding the wash-water to the main filtrate. In order to convert the calcium ethyl sulfate to sodium ethyl sulfate, add a concentrated aqueous solution of sodium carbonate cautiously drop by drop to the well-stirred filtrate until a drop of the latter withdrawn on a glass rod is just sufficiently alkaline to turn red litmus-paper blue. Then filter the solution at the pump, and wash the residual calcium carbonate again with a small quantity of water. Evaporate the filtrate on a water-bath until a drop withdrawn on a rod crystallizes on cooling: then allow the solution to stand until almost cold, and finally chill it thoroughly in ice-water. (If the ice-water cooling is omitted, large well-developed colorless crystals of sodium ethyl sulfate will finally separate.) Filter off the crystals at the pump, drain, and dry over calcium chloride in a desiccator. Yield about 12g. To obtain a second (but necessarily less pure) crop of the sulfate, evaporate the filtrate further on the water-bath, and cool as before.
Method 2 [4]
Two moles of absolute ethanol (92 grams) is slowly dripped into a beaker containing one mole of 20% Oleum (H2SO4 containing 20% SO3), adjusting the rate so that the temperature is maintained at 45°C. When all the ethanol is added, the solution is neutralized with anhydrous sodium carbonate (Na2CO3), care being taken for the evolution of carbon dioxide. Yield 85% of theory.
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2. DO SOME Phenyl-2-Nitropropene
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Synthesis of Phenyl-2-Nitropropene
(from:
https://www.thevespiary.org/rhodium/Rhodium/chemistry/phenyl-2-nitropropene.html
)
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[ Back to the Chemistry Archive ]
Procedure (By Dreamer)
To 55 g (0.5mol) Benzaldehyde in a 500ml Flask were added 40 g (0.5mol) Nitroethane and 10ml Cyclohexylamine. All was refluxed for 6h on a water bath. The result were 2 layers. One orange layer at the bottom with phenyl-2-nitropropene and a clear layer at the top with cyclohexylamine and maybe a little bit (~1ml) of H20. 50ml of H2O were added and then sucked off with a pipette until the phenyl-2-nitro-propene crystallized (it crystallized when it came in touch with air in presence of 15ml H2O). I added 200ml 95% denaturated ethanol to the orange crystals. The color of the now needle-like crystals changed from orange to white-yellow. The crystals were filtered. Yield 65 g, 78% of theory.
(YOU CAN EXCHANGE THE CATALYSATOR CYKLOHEXYLAMINE AGAINST AMMONIUM ACETATE..)
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3. REDUCE P2NP!
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(from:
https://www.thevespiary.org/rhodium/Rhodium/chemistry/amph.urushibara.txt
)
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Urushibura Style Amphetamine
by Ritter
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First of all many thanks go to CHEM_GUY for his continuous urging of the Hive
community to try Urushibara Nickel reduction on phenylnitropene. This reduction
turned out to be easier than any so far encountered. This is not based on any of
the excellent references pertaining to Urushibara that have been mentioned on
the hive, only chem_guys postings!
Procedure:
Dissolve 4.0g Nickel Chloride hydrate (light green crystals) in 75 ml 95%
ethanol w/ mag stirring and warming to 50'C. After salt is dissolved remove stir
bar and add 1ml water and 1ml conc. HCl. [1] While solution at 50'C slowly add
5g regular Reynolds wrap torn up into .25 x 1.0in strips in 1g portions with
manual stirring. The aluminum will SLOWLY react with the nickel salt forming the
metal Ni(s) through metathesis as a dark grey chunky powder which settles to the
bottom. A gentle effervescence of hydrogen occurs during reaction. Add aluminum
at a rate that maintains a steady effervescence and keeps temperature roughly in
the 50' range. Note this may take up to two hours!
At the end of Al addition all green color from nickel salt should be discharged.
If any color remains add another gram of aluminum and wait for soln to clear.
Precipitated Nickel powder was added to 100ml 20% NaOH soln and manually stirred
at 60'C for 30 min. Excess NaOH is decanted and nickel is washed with 5 x100ml
aliquots of distilled water to remove excess base. At this point Urishubara
nickel catalyst is prepared and ready for reduction.
Dissolve 5g pure phenylnitropropene in 50ml Ethanol and add to Ni solution [2].
Now slowly add 3ml conc. HCl [3] and 1 gram shredded aluminum w/ manual
stirring. Aluminum will slowly dissolve with a more vigorous effervescence of
hydrogen than the first step. Maintaining good stirring with a glass stirring
rod is essential in beginning. Attempted magnetic stirring will result in
frustration because nickel is ferromagnetic and will stick to stirbar preventing
surface area exposure necessary for reduction. After aluminum is dissolved add
three more milliliters HCl and one more gram Al. Repeat adding acid and Al until
10 grams Al and about 30ml HCl has been added. Aluminum reacts slowly. Expect
addition to take about six hours, longer if temp falls below 50’C. Constant
stirring towards end is not necessary, just give mix a good stir occasionally.
After all aluminum is added and mostly decomposed slowly pour in a soln of 30g
NaOH in 100ml H20 with careful stirring. Wear goggles and be careful! Base
neutralization is highly exothermic! In 30 minutes all aluminum sludge will
solvate into bottom aqueous layer and a nice orange alcohol layer reeking of
amine will settle out on top. Nickel is not dissolved by the NaOH so it will
remain floating around between the two layers but this does not present a major
problem. After all, it’s not poisonous like mercury or anything! Now decant off
the top orange organic layer and distill off alcohol down to a orange stinky
syrup completely different smelling than the P2NP. Dissolve these goodies in
acetone and slowly add sulfuric acid to precipitate the amine sulfate.
Voila!!!!!! about 3 grams light yellow amphetamine sulfate.
[1] Addition of water and acid found to be necessary to initiate rxn between
NiCl2 and Al.
[2] When nitropropene was added to NiCl2 soln before conversion to Ni powder
was complete some polymerization occurred greatly reducing yield.
It seems essential to add P2NP to rxn after Ni is fully precipitated.
[3] Use of Sulfuric acid produced inferior results causing polymerization of
P2NP to red tar.
Increasing Yield: Use overhead mechanical stirring to keep nickel catalyst
better suspended during reduction. Re-extract aqueous NaOH/Al
layer w/ toluene and work up in standard manner. Use larger
amount of nickel catalyst and more aluminum for H2 generation.
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4. ENJOY!!!!
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