Easiest way to amphetamine in the kitchen+Fentanyl

[malvaxman]

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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[PrimoPyro]

[pissy_rant]

Why does everybody enjoy reposting what is already documented? What good purpose does this serve?

1.You took this from Rhodium's site, meaning the links and a short description would suffice just dandy.

2.Much of the information on Rhodium's site was taken from Hive discussions! This info is already here! Why repost it?

It is a waste. Links to Rhodium's site with a description of what you are talking about, and post numbers relevant to the topic are all you need. You do not need to repost the entire writeup.


As a side-note, I could not agree more, unless someone has a source of PPA, which is easier to make into amphetamine than this of course. This process is my absolute number one favorite idea for producing amphetamine from scratch.

Amphetamine itself may suck as a stimulant, but there are fucking awesome compounds that can be made from it, that are harder to make when starting from methamphetamine. (although not impossible to do from meth.)

[/pissy_rant]

                                                  PrimoPyro
Vivent Longtemps La Ruche!

[malvaxman]

There is a purpose in posting it all in one post. I am sure I will make many newbees happy and many bees happy by the fact that newbees will maybee ask fewer stupid question.
All the texts and methods at Rhodiums are difficult to orientate in, specially for newbees and persons without chemisty education.
Many methods which are high yeilding use exotic chemicals and expensive to obtain equipment..
Now when some newbee asks "How do I do amphetamine at home the easiest way", you can link this post..

Now a question for you Primopyro, you write; "Amphetamine itself may suck as a stimulant, but there are fucking awesome compounds that can be made from it".
 Which are those "awesome compounds" you are thinking about, that outclass amphetamine and even meth???  

[PrimoPyro]

They are not stimulants.
Vivent Longtemps La Ruche!

[malvaxman]

So what compounds which could be made from amphetamine do you enjoy so much???

[PrimoPyro]

I do not enjoy their use, but I do enjoy reading about them. They would be the longer lasting amphetamine based fentanyl analogs. Standard fentanyl is has four major parts to the molecule.

1.The phenyl-alkyl group, that is attached to the N-piperidine structure.

2.The piperidine structure.

3.The anilino structure attached to the 4-piperidine.

4.The propionamide portion of the anilino.

Normally, the first portion is a phenethyl group. There are multiple ways of making the second level precursor: the phenyl-alkyl-piperidone. One way involves chaining the phenylalkyl bromide with piperidone.

Another way uses the phenylalkylamine, and constructs the piperidone ring around it. Phenethylamine would be used in this method as the amine, giving rise to phentanyl. If amphetamine were used, it would give rise to beta-methyl fentanyl I believe it is called by Drone 342, which may not be any more potent, but certainly lasts longer, like all amphetamine versions of phenethylamine drugs.

beta-methyl-3-methylfentanyl would be the strongest opioid I know of, with a dosage of a mere 60mcg for a 220lb (100kg) man, i.v. and it would last longer than the phenethyl version.

Sounds better than meth, no?

                                                     PrimoPyro
Vivent Longtemps La Ruche!

[Rhodium]

cis-3-methyl-fentanyl has an active dosage of 5-10 mcg (designer drugs directory) - where did you find the activity of cis-3,beta-dimethyl-fentanyl? Logically, it should be even stronger.

[obia]

what youre calling beta methyl fentanyl is called alpha methyl fentany AMF in the forensic business. Beta methyl would have the Me next to the phenyl group.
super potent fentanyl homologues could be most interesting if the problems with respiratory depression could be solved the only decent solution i could think of was to use a cut containing small amounts (sub active for a normal dose)but in an od situation enough would be present to prevent death its no good having naloxone/naltrexone unless someone else is there to inject it.
A better solution is to create an euphorient without the other effects, which unfortunately is exactly the opposite to what a pharmaceutical company wants, (how many compounds with the undesirable side effect of creating extreme euphoria but poor analglesia are lurking in pharm company archives?) How about the fentantyl derivative with a methylene bridge across the piperidone portion. the analog with tryptamine replacing phenethylamine could also be entertaining, it would certainly be active.

[PrimoPyro]

malvaxman: Your rebuttal still doesn't explain why retyping it is better than posting links with a description to save space.

Rhodium: I make this assumption to cover my ass. I too think the amphetamine will have higher potency, but I have not read specifically so, so I stay with what I know for certain: amphetamines have longer action than phenethylamines, fentanyls included.

Obia: the stigma is the same the same the same. We're not talking about fentanyl being perfect, but the bottom line is that it is here here and now, not hidden in some future discovery. Its not perfect by any means, but the stigma around it is severely overrated.

Every time a fentanyl discussion arises, the only information to surface is warnings about disaster, etc. Never any real chemistry discussions. All questions are answered with, "Do something simpler first." and all topics on it are altered with negativity about its use.

I personally think this is because people dont have the answers to the questions, so they say what they know. They have heard these stories before, and heard others say its bad its bad its bad, its so dangerous, you'll kill yourself, be careful, you're not ready, try methadone, etc.

Did anyone ask for advice? No. Its a chemistry question. Answer the question. Enter the discussion. Dont have anything to add? Then shut the fuck up.

Obia, this most certainly not directed toward you. You have presented the data initially in the thread, which is good for first time readers, so dont think Im chewing you out, because Im not.

I think its about time for a new, good, fentanyl discussion. I wish Drone were here. He wouldnt listen to the "its dangerous, wha wha wha" bullshit either. All drugs are dangerous. End of story. Fentanyl has special conditions. Work in a glovebox.

Back to a useful discussion: Rhodium, in

Post 60132 (missing)

(Rhodium: "N-phenylethyl-4-piperidones via acrylates", Chemistry Discourse) you say that condensing phenethylamine with two equivalents of methyl methacrylate will give rise to 3-methyl piperidone. I assume this is a typo? Did you mean condense with one equivalent of the methyl methacrylate, and one equivalent of methyl acrylate? Would not two methyl methacrylate additions yield the 3,5-dimethyl-piperidone?

                                                    PrimoPyro
Vivent Longtemps La Ruche!

[Chromic]

Every time a fentanyl discussion arises, the only information to surface is warnings about disaster, etc. Never any real chemistry discussions. All questions are answered with, "Do something simpler first." and all topics on it are altered with negativity about its use.

Perhaps that's because the people who often engage in such topics don't have enough theoretical framework to get involved with such a conversation or lack the equipment and/or the reagents to perform the appropriate synthesis. However... I'm sure there's a few folk on the Hive who'd love to discuss it with you, unfortunately I'm one of the people who lack both the necessary framework and the necessary reagents, so I'll back out of this topic.  

P.S. We absolutely need people with a better knowledge of the chemistry than I to participate in this discussion and be able to put together a document such as the one Dal Cason put together for MDxA,

https://www.thevespiary.org/rhodium/Rhodium/chemistry/mda.dalcason.html

I enjoy reading conversations such as the one in this thread, but unfortunately my skills don't allow me to do anything more than follow along with the discussion. (that's why I said I'd back out, as further posts from me would just add clutter that you and I both don't want to read!)  

[PrimoPyro]

Of course, I understand that caution is adviseable Chromic. Im not some gung-ho idiot looking to make 40 tons of heroin. What I mean is that these warnings have their place, but they appear in places that they are not asked for, such as a synthesis of 4-piperidone for example.

A discussion where I could have learned something suddenly changes to "the dangers of fentanyl" and the thread dies of its own accord. Yes, that really pisses me off. Its like being beaten in the head with "Drugs are bad, mkay?"

Dont back out of a discussion if you have something to say. I certainly dont have any equipment to test these things, but I dont mind talking about them.

                                                   PrimoPyro
Vivent Longtemps La Ruche!

[Rhodium]

PP: I wondered where you found the dosage information for dimethylfentanyl (you say 60 mcg), as already 3-methylfentanyl is active at 5-10 mcg.

Your correction of my post regarding the michael addition is fully correct, and I have changed my original post to reflect this.

[PrimoPyro]

Rhodium, I am sorry, I had a typo in my post, I meant to say it is at least that potent.

Taken from:

https://www.thevespiary.org/rhodium/Rhodium/chemistry/carfentanil.html

"For oxalate salt (carfentanyl) ED50 = 0.0006 mg/kg i/v, this mean that for 100-kg body you need only 0.06 mg. FYI, for 3-methylfentanyl (ED50=0.00058 mg/kg i.v.) look up is synthesis in J. Med. Chem. vol 17, No. 10, p. 1047 (1974)."

This is from your carfentanyl synthesis paper on your site. 3-methyl fentanyl is stated to have an effective dose of 0.06mg, which is of course 60mcg.

It is only logical that the even more powerful amphetamine analog would be at least that potent as well, as well as my assumption of longer activity. I had meant to imply that it should be at least as potent as 3-methylfentanyl, the dosage of which I got from your site.

Jesus Christ! I am forgetting that I own certain books! I havent read The Designer Drug Dictionary in a long time! I forgot I even had it!    I should have looked there.

Rhodium, I wonder, is the activity of the 3,5-dimethyl-fentanyl less, or what is up with that? It would most certainly be easier to only have to use methyl methacrylate instead of methyl acrylate and methyl methacrylate. The methacrylate would produce the 3,5-dimethyl analog if it worked.

Also, would the methyl interfere with the michael addition? Doesn't the carboxyl end up in the 5 position, or is it the 2/6 position?

                                                    PrimoPyro
Vivent Longtemps La Ruche!

[Rhodium]

The carboxyl ends up next to the 4-keto group after cyclization, before decarboxylation (that is the 3/5/"ortho" position). If making 3,5-dimethylpiperidones, the carboxy group would be tertiary instead of secondary, right? In that case the method would work very well for that analog in my opinion. I don't have any data on the corresponding fentanyl handy,but it should be in the patent literature.

[slappy]

3,alpha-Dimethylfentanyl is actually less potent than 3-Methylfentanyl. Again, you can't really combine the features of different Fentanyl's and expect a more powerful analouge. cis-(-)-3-Methylfentanyl is the most powerful 4-monosubstituted anilinopiperidine known. Carfentanil is the most powerful opiate that I am aware of, and both the 3-Methyl and alpha-Methyl homologes of it are less potent than the parent compound. Go figure.

Also, when considering the potency of 3-Methylfentanyl, you have to consider that when you make it, you actually have four isomers, and only one of those posesses the extreme potency.

An added benefit of making 4,4-Disubstituted Fentanyl analoges is that they don't show up on a toxicological screening.

[slappy]

Actually, there is one compound that I know to be more potent than Carfentanil. It is the Carfentanil skeleton, except with a -CH₂CH₂COOC(CH₃)₃ in stead of -CH₂CH₂Ph on the Piperidinyl Nitrogen. This compound is 1000's of times more powerful than Fentanyl.

You can find it in J. Med. Chem 1991 34(7), 2202-6

[Rhodium]

>1000x Fentanyl, that is right out sick - you'd get respiratory depression just by looking at that compound through a glass window... The N-substituent is tert-Butyl-propionate, right?

[PrimoPyro]

Could beta alanine { CH2(NH2)CH2COOH } be condensed with t-butanol and a dehydration agent like KHSO4 to its ester like normal carboxylic acids can?

The t-Bu ester of beta-Alanine would be the starting amine for the Michael Addition with methyl acrylate.

And for the other way, the condensation of the bromo compound with piperidone, one would need either 3-bromopropionic acid, or the t-Bu ester thereof.

Could one dehydrate 3-bromopropionic acid and t-butanol with KHSO4 or something similar, to the ester? Will the bromine interfere?

                                                     PrimoPyro
Vivent Longtemps La Ruche!

[Rhodium]

That sounds like something you look up in the chemical literature instead of thinking it up yourself. I would. I always perform a www.google.com and www.scirus.com search for all the synonyms of small molecules I want to know the synthesis for - it is generally much faster than thinking, and it also verifies any ideas you can think of. Half of the questions I don't know the answer for off the tp of my head can be answered with those search engines.

[slappy]

Let's put it this way, Carfentanil which is over 100x Fentanyl have a ED₅₀ of 520ng/kg, and according to this paper, the N-tert-Butyl Propionate derivative has a ED₅₀ of 28ng/kg. So yes you would probably suffer respitory depression just by looking at it behind glass.

Interestingly enough, the U.S.Army holds multiple patents on the synthesis of Carfentanil. It seems as though they had quite an interest in it around the late 70's through the 80's, perhaps for use as a chemical warfare agent?