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Fentanyl Synthesis

Needtolearn

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Fentanyl kills! Never try to synthesize it, much less use it!

Synthesis of Fentanyl


Fentanyl and its analogs are among of the most powerful opiate agonists, but their synthesis are often hard. Here is a synthesis of Fentanyl which can be easily adapted for the other analogs (para-Fluoro-Fentanyl, alpha-Methyl-Fentanyl).

This procedure is not theoretical and have been tested and improved many times over. This synthesis is conducted at room temperature so you don't need any special apparatus.

Fentanyl is a very interesting component for underground chemistry because one gram of pure fentanyl is equivalent of 100 g of very good street heroin.

Principle

The precursor used is N-Phenethyl-Piperidone (NPP) which can be easily synthesized from Piperidone and Phenethyl-tosylate or Phenethyl-bromide through a simple SN2 mechanism.The NPP is reacting with Aniline giving the Imine derivative which is reduced to the 4-Anilino-N-Phenethyl-Piperidine (4-ANPP). The 4-ANPP is then reacted with Propionyl Chloride giving Fentanyl which is then purified.

Experimental





N-Phenethyl-4-piperidone (NPP)


N-alkylation of 4-piperidone can be done in PTC conditions - and no need to isolate your piperidone as free base. Add to one liter of acetonitrile 3 mole finely powdered potassium carbonate, then add 10 g of PTC catalyst - TBAB or TEBA, or just polyethylene glycol-400. Stir this suspension 15 min at 50-60°C, and then add in little portions your 4-piperidone hydrochloride, watching that the CO2 evolution wasn't too vigorous. Stir another hour at 50-60°C, and then add phenethylbromide dropwise , and stir 15-20 h at mild reflux. Then cool, and filter off inorganic salts - if filtration goes too slowly, add to suspension some (30-40 ml) saturated sodium sulphate solution, this makes the sticky precipitate granular and filterable.

Yield almost quantitative (trust me), and no distillation needed - as result you have slightly yellow solid with mp 60°C.

a. Synthesis of NPP N-Phenyl-Imine

10 mmole of NPP is dissolved in a minimal volume of aniline (about 5-6 ml), then 1 gr of 4A Molecular Sieves is added. The mix is really gently stirred (so that the Molecular Sieves aren't destroyed by the agitation) with a magnetic stirrer for about 24 h at room temperature.

The conversion have repeatedly been calculated with MS and is more than 99%, so the next phase can be conducted without any purification.

b. Synthesis of the ANPP

The reaction mixture from the previous step is filtered from the molecular sieves which are rinsed with 2×2ml THF, the filtrate and washings are poured into a 50 ml flask, whereupon 20 ml dry Methanol is added, and the mix is stirred.

About 1-1.5 g of Sodium Borohydride is very slowly added to the mixture at room temperature, and the mix is stirred for about 2 h. The conversion into ANPP is checked with any method and if not completly reduced, add slowly another 0.5 g NaBH4 and stir for one more hour. When the conversion into ANPP is complete (over 95%), evaporate the Methanol and THF under vacuum.

The residual mass consists of aniline, excess NaBH4 and ANPP complexed with borane. Pour 50 ml of water into the flask, then destroy the complex by the slow addition of a small quantity of concentrated HCl (35%) until pH ~1, then the mix is well stirred for another hour. Now 50ml of a saturated NaCl solution is added to the mixture, and after about 10 min, a solid mass precipitate.

Separate the solid from the liquid with a filtration and keep the solid (this is ANPP hydrochloride) after washing it with a little saturated NaCl solution. Add another 50ml of saturated NaCl solution and place the mix in the fridge (at about 2°C) and wait 2-3 h. If there is more precipitate, filter the solution and add the solid to the first crop. The solid mass is ANPP which must be treated.

Dissolve the solid in about 60ml water and 2N NaOH until pH > 12.5, then extract with 3×15ml CH2Cl2. Wash the CH2Cl2 phase with 5 ml water, and evaporate the solvent in vacuum. The residue is an oily yellow-orange liquid which spontaneously crystallizes, consisting of ANPP pure enough for the next step.

The overall yield of ANPP is about 50-80%. The main loss of yield is during the purification process because the separation process between the excess of Aniline and ANPP is not optimized. There are perhaps some solutions to this, which will be discussed in the optimization and discussion chapter.

c. Conversion of ANPP to Fentanyl

10 mmol ANPP is dissolved in about 8 ml of dry, pure pyridine with stirring, and then 12 mmol of propionyl chloride is added dropwise to the reaction mixture at room temperature. The reaction is exothermic and the temperature should be controlled by carefully adjusting the addition rate, and it must be kept between 30-60°C at all times. When all the propionyl chloride is added, the reaction mixture is stirred for about one hour at room temperature.

Check the conversion with any suitable method (TLC/GC) and if not complete add another 1 mmol of propionyl chloride. Normally the conversion should be complete after the first operation but if there is too much aniline left from step A, you need more Propionyl Chloride.

The reaction mix is then poured into 80 ml water with stirring, and concentrated HCl (~35%) is added dropwise until pH < 1.5. This operation can be done with another procedure as follows: Prepare 80 ml of 2N HCl and simply pour the reaction mix into this solution. This results in the pyridine and the Fentanyl turning into their respective hydrochloride salts. The solution is then stirred for about 30 min. Pyridine·HCl is not soluble in CH2Cl2, while the nonpolar Fentanyl·HCl is. Extract the solution with 3×20ml of CH2Cl2, then wash the pooled organic extracts with 2×10ml saturated NaCl solution.

The solvent is evaporated under vacuum, and a yellow mass is formed which consists of Fentanyl hydrochloride contaminated with a small quantity of propionanilide, which was formed by the action of propionyl chloride on residual aniline from step A. 10-15 mL acetone is now added, and a white powder forms, which is Fentanyl·HCl. Filter the solid and wash it with a small quantity (2×3 mL) of acetone.

The Fentanyl Hydrochloride is now pure enough for use (>99.5%), the yield of this step exceeding 90%! If it would still be impure (it was never the case for me) you can purify it by recrystallisation from hot acetone.

Dilution of fentanyl powder

The pure Fentanyl can not be used as is, because it's much, much too strong and MUST be diluted, else there will be a lot of overdoses!

The following procedure gives a white heroin wich is the same strength as very good (30%) street heroin.

100mg of Fentanyl·HCl is dissolved in 2ml of methanol. Weigh up 10g of lactose and warm it to about 60-70°C into a large dish with a hotplate. Add the methanolic solution of Fentanyl dropwise at regular intervals into the warm lactose for a good pre-mix. Wait until all the methanol is evaporated and mix thoroughly. This is crucial because if this is not thoroughly mixed, there will be a part of the Lactose without Fentanyl and part of the Lactose with too much Fentanyl, possibly causing dramatic overdoses!

This type of Heroin was used and sold during a year, and the feedback of the consumers was very good. The consumers were very happy and didn't want the usual brown Heroin anymore. So be careful, some people (the Mafia and other dealers) will perhaps turn very jealous!

DON'T USE and DON'T SELL pure Fentanyl HCl, this is a very toxic material which will cause many overdoses if not diluted!

Optimization and discussion

The overall yield of this synthesis is about 50-80% and the main loss of material occurs during the purification of ANPP in step B. There are perhaps other alternatives for the separation of Aniline and ANPP (recrystallisation, distillation). I think a good solution is extracting the Aniline and ANPP together and separate them with the evaporation of Aniline under vacuum, then recrystallize the ANPP in a suitable solvent.

Para-Fluoro-Fentanyl can be synthetised with this procedure using p-fluoroaniline instead of plain aniline, but the purification process must be adapted.

The very powerful alpha-Methyl-Fentanyl can also be synthetised with this method using N-(2-Phenylpropyl)-Piperidinone which can be synthetised from 1-Phenyl-2-Bromopropane and Piperidinone or other methods. The 1-Phenyl-2-Bromopropane is used in clandestine manufacture of amphetamine, and the procedure of the synthesis of this compound can be easily adapted for the creation of N-(2-Phenylpropyl)-Piperidinone or the NPP (N-Phenethyl- Piperidinone).

Fentanyl is a very good and powerful opiate but there are some remarks:

  • Fentanyl is very addictive, much more than simple Heroin, the regular users of this synthetic white Heroin I described were heavily addicted.
  • The risk of overdose is really high, even with the dilution i described before, so test your stuff before selling it!
  • The duration of the effects is a little shorter than with normal Heroin.
 

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MadHatter

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Hmm. I guess this synth had to pop up here eventually. But this is pure poison. Never ever undertake this synth without rigorous PPE, a coworker and access to naloxone.
 

Needtolearn

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i absolutly agree dont even think about doing this unless you know 100% what you are doing. if done correctly this is so potent that particle pollution and every surface it has had contact with can kill you if you touch it with bare hands. always remember A few grains can be enough to kill you!!!!!!!
 

Teck Tonik

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Hmm. I guess this synth had to pop up here eventually. But this is pure poison. Never ever undertake this synth without rigorous PPE, a coworker and access to naloxone.
DocXLook I get why this stuff is looked down upon but if it's used responsibly it can also be a life savor! I've been opiod dependent for 11 years now and since I started using fentanil i can finally stay well enough to get my shit together. I don't nod much and I've never had an overdose thus far seems to me that this drug could he dangerous but also could be the cure to opiod dependacy in the future in a more liberal sense! By using fentanyl it's almost as if my life I back in a lot of ways also I don't use a needle anymore because smoking it is fine! Honestly i couldn't fit the long list of pros that exist for this drug in this comment thread , at the same time the list of cons is right behind it in length so it's all perspective I suppose.......
 

Teck Tonik

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i absolutly agree dont even think about doing this unless you know 100% what you are doing. if done correctly this is so potent that particle pollution and every surface it has had contact with can kill you if you touch it with bare hands. always remember A few grains can be enough to kill you!!!!!!!
NeedtolearnThanks for the information brotha!
 

Saul

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this stuff is the devil ! I dont like it that this is allowd to share on braking bad . this is breaking dead
 

MadHatter

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Look I get why this stuff is looked down upon but if it's used responsibly it can also be a life savor! I've been opiod dependent for 11 years now and since I started using fentanil i can finally stay well enough to get my shit together. I don't nod much and I've never had an overdose thus far seems to me that this drug could he dangerous but also could be the cure to opiod dependacy in the future in a more liberal sense! By using fentanyl it's almost as if my life I back in a lot of ways also I don't use a needle anymore because smoking it is fine! Honestly i couldn't fit the long list of pros that exist for this drug in this comment thread , at the same time the list of cons is right behind it in length so it's all perspective I suppose.......
Teck TonikWell, this is a forum for drug production, at least this part of the forum. And when you're producing fentanyl, carfentanyl or some other fentanyl analogue you're putting yourself at risk. If you're not 100% sure of what you're doing, you're putting a lot of more people at risk also. This is not about your personal experience, it's actually not very interesting in this context.
If you're dabbling with pure fentanyl in the production line, it's like juggling a rattlesnake. The transdermal route is widely overstated, but to mistakenly breathe in the product can lead to a relatively quick and lethal intoxication. If you're not 100% sure about how to dilute the stuff for end users, you run the risk of killing them also.
 

Teck Tonik

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Well, this is a forum for drug production, at least this part of the forum. And when you're producing fentanyl, carfentanyl or some other fentanyl analogue you're putting yourself at risk. If you're not 100% sure of what you're doing, you're putting a lot of more people at risk also. This is not about your personal experience, it's actually not very interesting in this context.
If you're dabbling with pure fentanyl in the production line, it's like juggling a rattlesnake. The transdermal route is widely overstated, but to mistakenly breathe in the product can lead to a relatively quick and lethal intoxication. If you're not 100% sure about how to dilute the stuff for end users, you run the risk of killing them also.
DocXI'm not going to pretend to know what I'm doing doing try to produce it myself, my friend on the other hand is a chemist and I'd be interested to see what he thinks of this. If it's possible to create this safely and he's confident he can then it would help my addiction because at the end of the day I'm just tying to function in a society that's against me ar every turn. I get its dangerous and I get it harms others but that's why safety precautions are important.
 

summer_child

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You can also synthesize NPP by reacting phenethylamine with 2 moles of methylacrylate.
 

Bill Cosby

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Could someone post a list of lab equipment needed for this?
 

eduardo salamanca

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I've been opiod dependent for 11 years now and since I started using fentanil i can finally stay well enough to get my shit together.
Teck TonikIf you want to get out of an addiction you should really try using ketamine. There have been various studies proving that ketamine helps people quit drinking among other habits. There is even a synthesis on this forum, if you want to make it yourself.
 

BongMan

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Could someone post a list of lab equipment needed for this?
Bill Cosby
first you need PPE Kit with high level GAS mask with proper cartridge , and cant perform in kitchen like clandestine lab, it is very dangerous even mist of this substance can kill you better not try to perform ,if you are not good in laboratory practice..
 

Bill Cosby

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I have a 3M full face respirator, 2091 filters, an AAMI level 4 PPE suit, shoe covers, and gloves. I believe those should do the job but I just want to make sure of course.
 

MadHatter

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It's not just a question of equipment, also a question of work flow. Safe handling of reagents and byproducts, good ventilation and so on. But gloves, coat, respirator and a fume hood is a minimum. Then you have to think about things like how you remove the gloves and respirator when you're done, what you do with them then, how you clean your equipment and so on. You're handling an extremely toxic chemical if you manage to get the final product right, and there are thousands of ways it could end up on your fingers or in your airways. That's why you should also have naloxone nasal spray or injections available. If you start to feel dizzy or sleepy it's really only a matter of minutes before you potentially loose consciousness. It's like juggling a rattlesnake.

Also, if you manage to do the synth and have the pure product, you need to dilute it in the right way to avoid hotspots in your mixture or unwanted high concentrations, or you'll kill the end user.

Or just don't do the synth.
 

Bill Cosby

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It's not just a question of equipment, also a question of work flow. Safe handling of reagents and byproducts, good ventilation and so on. But gloves, coat, respirator and a fume hood is a minimum. Then you have to think about things like how you remove the gloves and respirator when you're done, what you do with them then, how you clean your equipment and so on. You're handling an extremely toxic chemical if you manage to get the final product right, and there are thousands of ways it could end up on your fingers or in your airways. That's why you should also have naloxone nasal spray or injections available. If you start to feel dizzy or sleepy it's really only a matter of minutes before you potentially loose consciousness. It's like juggling a rattlesnake.

Also, if you manage to do the synth and have the pure product, you need to dilute it in the right way to avoid hotspots in your mixture or unwanted high concentrations, or you'll kill the end user.

Or just don't do the synth.
DocXAt risk of sounding naïve, if I have a college chemistry degree, a lot of lab experience, access to the necessary lab equipment, someone on standby with naloxone, and will put a ton of thought into safe handling during dilution. So if you still think there is a high risk of me accidentally killing myself, how are people in the Baltimore projects diluting pure fentanyl successfully? The synth is one thing, but regarding handling the product, people in the projects are much less prepared and much less equipped, and there are countless people down there diluting pure fentanyl. And I appreciate the response and your concern. I am simply curious about the latter question.
 

MadHatter

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At risk of sounding naïve, if I have a college chemistry degree, a lot of lab experience, access to the necessary lab equipment, someone on standby with naloxone, and will put a ton of thought into safe handling during dilution. So if you still think there is a high risk of me accidentally killing myself, how are people in the Baltimore projects diluting pure fentanyl successfully? The synth is one thing, but regarding handling the product, people in the projects are much less prepared and much less equipped, and there are countless people down there diluting pure fentanyl. And I appreciate the response and your concern. I am simply curious about the latter question.
Bill CosbyWell, how do you know there AREN'T a lot of incidences in the clandestine labs? If someone crooks in a ghetto lab, I would think they're simply dragged into an alley and end up reported as one of those extremely common fentanyl overdoses (*wink wink) that litters the back alleys of most major cities.

Also, I think the best safety precaution when working with a substance like this is to work in a team and have naloxone handy. That will go a long way. An overdose of fentanyl is actually quite easy to handle, thanks to the near-magical effect of naloxone. But not if you're alone and unconcious.

But if you have a lot of lab experience, that's good for you and goes a long way! Fentanyl doesn't absorb particulary quickly transdermally, so the dangers of that is widely overrated. Inhalation of atomized powder would however be directly life-threatening.
 

darkmatter7

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I used to IV fent analogues, and I was pretty good at not dying, but then one day I did too much, and there's just no time for naloxone - as soon as the needle is pressed down, that is my last memory (before waking up to a naloxone shot with <20% blood oxygen saturation levels)
 

MadHatter

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Yes, and this is the main reason to not synthesize fentanyl or its analogues for uncontrolled consumption. People WILL die from them. Opiates are what kills people, no other drugs, and fentanyl is an absolute murderer. By synthing it, you will be accessory to the fact. Period.
 

Bill Cosby

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I will say, the past majority of the stuff on the street is extremely poorly homogenized, even harder to do with an even more potent analogue. I do believe I could provide something free of hot spots, and if people got a hold of my stuff rather than the stuff darkmatter7 mentioned, I think I could actually save some lives.
 

Bill Cosby

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Not to mention they are cutting the fentanyl on the street with benzos now....
 
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