One-Pot Fentanyl Synthesis

[OrgUnikum]

The synthesis and preliminary pharmacological evaluation of the racemic cis and trans 3-alkylfentanyl analogues
Journal of the Serbian Chemical Society. 69 (7): 511–26. (2004) doi:10.2298/JSC0407511

https://doiserbia.nb.rs/img/doi/0352-5139/2004/0352-51390407511I.pdf

Great article, lots of useful bits and pieces. Straight from Wikipedia btw.

I want to add a caveat (be careful) regarding F synths in special and drug synths in general as they can be found in scientific articles. Guys, those people are not completely daft if if they are the publishers of the journals are not. You will not find a well working easy synthesis of drugs there even if it looks like it. Those articles (except those where special equipment or reagents are needed) are all booby-trapped with misinformation which is supposed to be obvious to other scientists but not to the person who just wants a recipe for cooking drugs. Well, in reality most of the other scientists don't see those traps but well, thats probably a second purpose.
Some examples:
The Leuckart and making Amphetamine with it is old, so very old but already in 1944 they just left this out or just lied about it really works in special about the hydrolysis step.
All the F synths staring with the piperidone which is reacted to NPP in one way or another, all talking 90% yield and up and everybody who tries it gets some hard resin instead? Thats done on purpose, it is obvious that piperidone if not protected will just react with itself as it has a ketone and an amine group. The only synths they mention with protected piperidone is the benzylated kind which needs Pd/C for deprotection. Also be aware that many Indian articles are just made up stuff to give them a reason to pretend they have a own synthetic pathway to certain drugs as thats whet they need to copy those by Indian patent law.
Super easy Ketamine synths from China. First the Chinese are exaggerating yields like nobody else, for some reason the just MUST do it. And they often publsih upscale methods, whats nice if they were not a little bit missing to really work. As those synths are worth real money in production its more advertisement where they say "we have something great - contact us to make a deal for the real optimized method". Often. Not always.
Ephedrine Biosynth from Sydney University Australia. Those guys even admitted in an interview that they designed their publications and patents in a way nobody without very special knowledge can make ephedrine using those. THey even boasted in an interview how they fooled somebody who contacted them for help in the matter and finally turned him in to the police but not before they made him start and get far enough to cop a really serious sentence. They were actually proud the assholes.

Goes on and on.

Just a reminder.

 

[testint]

The synthesis and preliminary pharmacological evaluation of the racemic cis and trans 3-alkylfentanyl analogues
Journal of the Serbian Chemical Society. 69 (7): 511–26. (2004) doi:10.2298/JSC0407511

https://doiserbia.nb.rs/img/doi/0352-5139/2004/0352-51390407511I.pdf

Great article, lots of useful bits and pieces. Straight from Wikipedia btw.

I want to add a caveat (be careful) regarding F synths in special and drug synths in general as they can be found in scientific articles. Guys, those people are not completely daft if if they are the publishers of the journals are not. You will not find a well working easy synthesis of drugs there even if it looks like it. Those articles (except those where special equipment or reagents are needed) are all booby-trapped with misinformation which is supposed to be obvious to other scientists but not to the person who just wants a recipe for cooking drugs. Well, in reality most of the other scientists don't see those traps but well, thats probably a second purpose.
Some examples:
The Leuckart and making Amphetamine with it is old, so very old but already in 1944 they just left this out or just lied about it really works in special about the hydrolysis step.
All the F synths staring with the piperidone which is reacted to NPP in one way or another, all talking 90% yield and up and everybody who tries it gets some hard resin instead? Thats done on purpose, it is obvious that piperidone if not protected will just react with itself as it has a ketone and an amine group. The only synths they mention with protected piperidone is the benzylated kind which needs Pd/C for deprotection. Also be aware that many Indian articles are just made up stuff to give them a reason to pretend they have a own synthetic pathway to certain drugs as thats whet they need to copy those by Indian patent law.
Super easy Ketamine synths from China. First the Chinese are exaggerating yields like nobody else, for some reason the just MUST do it. And they often publsih upscale methods, whats nice if they were not a little bit missing to really work. As those synths are worth real money in production its more advertisement where they say "we have something great - contact us to make a deal for the real optimized method". Often. Not always.
Ephedrine Biosynth from Sydney University Australia. Those guys even admitted in an interview that they designed their publications and patents in a way nobody without very special knowledge can make ephedrine using those. THey even boasted in an interview how they fooled somebody who contacted them for help in the matter and finally turned him in to the police but not before they made him start and get far enough to cop a really serious sentence. They were actually proud the assholes.

Goes on and on.

Just a reminder.

OrgUnikumMisleading papers to protect products are very common they know all the ways to fail and even disaster which they are not kind enough to provide the nerve

 

[testint]

The synthesis and preliminary pharmacological evaluation of the racemic cis and trans 3-alkylfentanyl analogues
Journal of the Serbian Chemical Society. 69 (7): 511–26. (2004) doi:10.2298/JSC0407511

https://doiserbia.nb.rs/img/doi/0352-5139/2004/0352-51390407511I.pdf

Great article, lots of useful bits and pieces. Straight from Wikipedia btw.

I want to add a caveat (be careful) regarding F synths in special and drug synths in general as they can be found in scientific articles. Guys, those people are not completely daft if if they are the publishers of the journals are not. You will not find a well working easy synthesis of drugs there even if it looks like it. Those articles (except those where special equipment or reagents are needed) are all booby-trapped with misinformation which is supposed to be obvious to other scientists but not to the person who just wants a recipe for cooking drugs. Well, in reality most of the other scientists don't see those traps but well, thats probably a second purpose.
Some examples:
The Leuckart and making Amphetamine with it is old, so very old but already in 1944 they just left this out or just lied about it really works in special about the hydrolysis step.
All the F synths staring with the piperidone which is reacted to NPP in one way or another, all talking 90% yield and up and everybody who tries it gets some hard resin instead? Thats done on purpose, it is obvious that piperidone if not protected will just react with itself as it has a ketone and an amine group. The only synths they mention with protected piperidone is the benzylated kind which needs Pd/C for deprotection. Also be aware that many Indian articles are just made up stuff to give them a reason to pretend they have a own synthetic pathway to certain drugs as thats whet they need to copy those by Indian patent law.
Super easy Ketamine synths from China. First the Chinese are exaggerating yields like nobody else, for some reason the just MUST do it. And they often publsih upscale methods, whats nice if they were not a little bit missing to really work. As those synths are worth real money in production its more advertisement where they say "we have something great - contact us to make a deal for the real optimized method". Often. Not always.
Ephedrine Biosynth from Sydney University Australia. Those guys even admitted in an interview that they designed their publications and patents in a way nobody without very special knowledge can make ephedrine using those. THey even boasted in an interview how they fooled somebody who contacted them for help in the matter and finally turned him in to the police but not before they made him start and get far enough to cop a really serious sentence. They were actually proud the assholes.

Goes on and on.

Just a reminder.

OrgUnikumRemember how they roasted David Nichols when the nbome came out he's forced to no longer publish

 

[The_Real_Gus_Fring]

WARNING: Fentanyl is extremely dangerous. Do NOT ATTEMPT this synthesis without naloxone present!
DISCLAIMER: This method does not produce high purify fentanyl (avg. is 13.6%, range 0.2% to 36.4%)

The original paper talking about this procedure can be found here.

Fentanyl is a very powerful opioid, much more powerful than both morphine and heroin.
View attachment 13084

The procedure listed below is a one-pot synthesis. It is attractive to the clandestine chemist due to it's possibility to be done in 3 steps all at room temperature. The only caveat is the requirement of N₂ gas.

The reaction scheme is shown below:
View attachment 13085


To a stirred suspension of 4-piperidone hydrochloride (15.36 g, 0.1 mol) in dichloroethane (450 ml), triethylamine (27.87 ml, 0.2 mol) and phenylacetaldehyde (11.17 ml, 0.1 mol) were added and stirred for half an hour at room temperature under N2. Thereafter sodium triacetoxyborohydride (30 g, 0.14 mol) was added to the reaction mixture with continuous stirring. Reaction mixture was further stirred for 24 h. Aniline (9.12 ml, 0.1 mol), acetic acid (11.53 ml, 0.2 mol) and sodium triacetoxyborohydride (30 g, 0.14 mol) were then added and again stirred for 24 h. Propionyl chloride (26.16 ml, 0.3 mol) was then added dropwise and the mixture was stirred for 2 h. The reaction mixture was then diluted with dichloromethane and washed with 4% aqueous sodium hydroxide solution followed by water. The organic phase was then shaken with 2N HCl. The organic layer was separated and the aqueous layer was extracted with DCM. Combined organic phase was dried over sodium sulfate and concentrated to give crude HCl salt of fentanyl. Crude product was recrystallised with acetone to give white powder of fentanyl hydrochloride. The salt was treated with 20% NaOH to give fentanyl which was recrystallised from petroleum ether (60–80°)

Yield: 13.44 g (40 %)
m.p. 82–83 °C.

Literature
The paper on synthesis of fentanyl in this manner can be found here.

mp_What does the nitrogen gas do? Why is it nessecary? Can this be done without the gas?

 

[BongMan]

What does the nitrogen gas do? Why is it nessecary? Can this be done without the gas?

The_Real_Gus_Fringit create inert atmosphere and prevent some side reactions you probably get pure product and high yields

 

[OrgUnikum]

it create inert atmosphere and prevent some side reactions you probably get pure product and high yields

BongManThis reaction will never yield pure product or high yields, it is impossible. 10%, maybe 20% if you are very lucky or skilled of highly impure product which has to be cut with some animal tranquilizer to be marketable. Or where and why did tranq come into existence?
Generally it is regarded as very bad business practice to kill ones customers, something whats only done by people so full of cocaine machismo and no tomorrow that they have lost all and any perspective or idea of something like "future". It is deranged to a point where obviously only measures like whats done in El Salvador provide salvation. Other implementations will soon follow and very soon they will just skip the hyper-prison for cheaper bullets. Everybody should be able to figure out what this means for the friendly mom and pop dealer - there will be no discrimination, if anybody thought the war on drugs was bad, brace yourself for the war on gangs*.

*if you think now: oh we have no such gangs here!, do not worry, you will have something what looks like very soon, like it was in Italy when the Brigado Rosso failed to terrorize the population sufficiently somebody did it in their name without asking. (Bologna train station bombing). So easy. So old. So efficient. Back then it cost us in Europe the bigger part of civil liberties, this now to come may cost your life.

 

[BongMan]

This reaction will never yield pure product or high yields, it is impossible. 10%, maybe 20% if you are very lucky or skilled of highly impure product which has to be cut with some animal tranquilizer to be marketable. Or where and why did tranq come into existence?
Generally it is regarded as very bad business practice to kill ones customers, something whats only done by people so full of cocaine machismo and no tomorrow that they have lost all and any perspective or idea of something like "future". It is deranged to a point where obviously only measures like whats done in El Salvador provide salvation. Other implementations will soon follow and very soon they will just skip the hyper-prison for cheaper bullets. Everybody should be able to figure out what this means for the friendly mom and pop dealer - there will be no discrimination, if anybody thought the war on drugs was bad, brace yourself for the war on gangs*.

*if you think now: oh we have no such gangs here!, do not worry, you will have something what looks like very soon, like it was in Italy when the Brigado Rosso failed to terrorize the population sufficiently somebody did it in their name without asking. (Bologna train station bombing). So easy. So old. So efficient. Back then it cost us in Europe the bigger part of civil liberties, this now to come may cost your life.

OrgUnikummate you are diverting this conversation in wrong way , first of all i am not dealer i am qualified chemist and did it for purpose and i made it 97-98 % pure and yes it was less pure around 60-70 % in synthesis but after purification once or twice we had 98 % pure i attached hplc report with date correction , if you are proper skilled and equipped you can do this in supervision of experienced chemist .

 

[OrgUnikum]

mate you are diverting this conversation in wrong way , first of all i am not dealer i am qualified chemist and did it for purpose and i made it 97-98 % pure and yes it was less pure around 60-70 % in synthesis but after purification once or twice we had 98 % pure i attached hplc report with date correction , if you are proper skilled and equipped you can do this in supervision of experienced chemist .

BongManOn the internet everybody can be anything he wants to be, not saying you are not a qualified chemist, like Sydney University qualified, well possible. Doesn't mean you have any idea what you are talking about, obviously not. Otherwise you would have addressed at least the easily fixed problems of this synth which are obvious from just looking at the molecules involved and reading the related Wikipedia articles.
Then you talk about purity. High purity can always be achieved as long there is any product which can be isolated. Mainly by column chromatography. But those who do this for the money do not purify anything at all. As it is hard to get anything isolated at all from this reaction as it is a ridiculous reaction scheme which MUST produce a lot of crap. Evil, polymere kind of crap. 1% to 10% of Fentanyl are in this crap. Extracting this is difficult. Solution: Don't extract at all but add some animal tranquilizer to compensate for the varying unknown amounts of maybe F in there and sell this as Tranq. And that is what people do. And that is why users are losing the fingers or toes or die. But look, this is not making and dealing drugs anymore, it is attempted or factual homicide.

 

[BongMan]

On the internet everybody can be anything he wants to be, not saying you are not a qualified chemist, like Sydney University qualified, well possible. Doesn't mean you have any idea what you are talking about, obviously not. Otherwise you would have addressed at least the easily fixed problems of this synth which are obvious from just looking at the molecules involved and reading the related Wikipedia articles.
Then you talk about purity. High purity can always be achieved as long there is any product which can be isolated. Mainly by column chromatography. But those who do this for the money do not purify anything at all. As it is hard to get anything isolated at all from this reaction as it is a ridiculous reaction scheme which MUST produce a lot of crap. Evil, polymere kind of crap. 1% to 10% of Fentanyl are in this crap. Extracting this is difficult. Solution: Don't extract at all but add some animal tranquilizer to compensate for the varying unknown amounts of maybe F in there and sell this as Tranq. And that is what people do. And that is why users are losing the fingers or toes or die. But look, this is not making and dealing drugs anymore, it is attempted or factual homicide.

OrgUnikummate if you seen i did not discuss any method i just talking about purity if you cant get pure product it doesn't mean it can not be,if you read this one pot synthesis they also mentioned pure product means it should be near above 70 % , i didn't mention any purification solution because this synthesis should not attempt by those who are layman or they think they can handle this devil what ever purity they got it is ok for them because danger and risk increase with increased purity , but yes if any one wants and can convinced me ,they are not layman and aware with all risk and danger and safely handle this may be i will guide him to make purer stuff , and yes this reaction never get even 10 % pure stuff if any one get 5-7% he will be lucky .

 

[Salvador]

WARNING: Fentanyl is extremely dangerous. Do NOT ATTEMPT this synthesis without naloxone present!
DISCLAIMER: This method does not produce high purify fentanyl (avg. is 13.6%, range 0.2% to 36.4%)

The original paper talking about this procedure can be found here.

Fentanyl is a very powerful opioid, much more powerful than both morphine and heroin.
View attachment 13084

The procedure listed below is a one-pot synthesis. It is attractive to the clandestine chemist due to it's possibility to be done in 3 steps all at room temperature. The only caveat is the requirement of N₂ gas.

The reaction scheme is shown below:
View attachment 13085


To a stirred suspension of 4-piperidone hydrochloride (15.36 g, 0.1 mol) in dichloroethane (450 ml), triethylamine (27.87 ml, 0.2 mol) and phenylacetaldehyde (11.17 ml, 0.1 mol) were added and stirred for half an hour at room temperature under N2. Thereafter sodium triacetoxyborohydride (30 g, 0.14 mol) was added to the reaction mixture with continuous stirring. Reaction mixture was further stirred for 24 h. Aniline (9.12 ml, 0.1 mol), acetic acid (11.53 ml, 0.2 mol) and sodium triacetoxyborohydride (30 g, 0.14 mol) were then added and again stirred for 24 h. Propionyl chloride (26.16 ml, 0.3 mol) was then added dropwise and the mixture was stirred for 2 h. The reaction mixture was then diluted with dichloromethane and washed with 4% aqueous sodium hydroxide solution followed by water. The organic phase was then shaken with 2N HCl. The organic layer was separated and the aqueous layer was extracted with DCM. Combined organic phase was dried over sodium sulfate and concentrated to give crude HCl salt of fentanyl. Crude product was recrystallised with acetone to give white powder of fentanyl hydrochloride. The salt was treated with 20% NaOH to give fentanyl which was recrystallised from petroleum ether (60–80°)

Yield: 13.44 g (40 %)
m.p. 82–83 °C.

Literature
The paper on synthesis of fentanyl in this manner can be found here.

mp_Hey, guys.
Can anyone explain this process clearly؟
What is the list of equipment needed for synthesis؟

I'd appreciate you helping.

 

[BongMan]

Hey, guys.
Can anyone explain this process clearly؟
What is the list of equipment needed for synthesis؟

I'd appreciate you helping.

Salvadoryou really want to try this synthesis.

 

[Salvador]

you really want to try this synthesis.

BongManYes، I want to synthesize in the Gupta way. But I don't know much about it.

 

[BongMan]

Yes، I want to synthesize in the Gupta way. But I don't know much about it.

Salvadormate i will not recommend to do this stuff if you are not skilled and aware with handling lab stuffs , Gupta's method seems look promising and easy but aldehyde form water molecules when react with amine and that will prevent addition , you need reactor and proper inert environment to perform this reaction i will recommend use molecular sieve in first step .......good luck

 

[abbalabba]

Some things are better left alone

 

[testint]

Some things are better left alone

abbalabbaAbsolutely

 

[BongMan]

this is we got after some try ...

 

[testint]

This is the current excuse to fuck your rights in the ass with a wire brush by any means rights be damned you wouldn't post child grooming methods so why post the boogie man of current date shit has been destroyed for less think fucker

 

[BongMan]

This is the current excuse to fuck your rights in the ass with a wire brush by any means rights be damned you wouldn't post child grooming methods so why post the boogie man of current date shit has been destroyed for less think fucker

testintchill mate its not for you .

 

[BongMan]

chill mate its not for you .

BongManwhat matters in this report is already there who cares what dated it was and yes it is a piece of shit for those who can not understand HPLC report i can understand their pain in the ass ,so please people keep ice pad near you

 

[testint]

It's the site I was puckered over not the info itself the papers to make sarin are out there but would posting them in a forum like this be helpful? Assuming someone's motives are we ? Insulting others intent ?

 

[BongMan]

It's the site I was puckered over not the info itself the papers to make sarin are out there but would posting them in a forum like this be helpful? Assuming someone's motives are we ? Insulting others intent ?

testintok mate i apologize if i hurt your sentiments but i didnt post any proven method i know this is devil and must be handle with responsibility.

 

[testint]

ok mate i apologize if i hurt your sentiments but i didnt post any proven method i know this is devil and must be handle with responsibility.

BongManThey Popped lizard labs because they thought he was doing something but the real reason was is big old mouth this is the last time I'll say this because people don't take it seriously shit even I sometimes don't take it seriously enough carry on my brother

 

[testint]

Dirty but probably passable

 

[Joker_55555]

WARNING: Fentanyl is extremely dangerous. Do NOT ATTEMPT this synthesis without naloxone present!
DISCLAIMER: This method does not produce high purify fentanyl (avg. is 13.6%, range 0.2% to 36.4%)

The original paper talking about this procedure can be found here.

Fentanyl is a very powerful opioid, much more powerful than both morphine and heroin.
View attachment 13084

The procedure listed below is a one-pot synthesis. It is attractive to the clandestine chemist due to it's possibility to be done in 3 steps all at room temperature. The only caveat is the requirement of N₂ gas.

The reaction scheme is shown below:
View attachment 13085


To a stirred suspension of 4-piperidone hydrochloride (15.36 g, 0.1 mol) in dichloroethane (450 ml), triethylamine (27.87 ml, 0.2 mol) and phenylacetaldehyde (11.17 ml, 0.1 mol) were added and stirred for half an hour at room temperature under N2. Thereafter sodium triacetoxyborohydride (30 g, 0.14 mol) was added to the reaction mixture with continuous stirring. Reaction mixture was further stirred for 24 h. Aniline (9.12 ml, 0.1 mol), acetic acid (11.53 ml, 0.2 mol) and sodium triacetoxyborohydride (30 g, 0.14 mol) were then added and again stirred for 24 h. Propionyl chloride (26.16 ml, 0.3 mol) was then added dropwise and the mixture was stirred for 2 h. The reaction mixture was then diluted with dichloromethane and washed with 4% aqueous sodium hydroxide solution followed by water. The organic phase was then shaken with 2N HCl. The organic layer was separated and the aqueous layer was extracted with DCM. Combined organic phase was dried over sodium sulfate and concentrated to give crude HCl salt of fentanyl. Crude product was recrystallised with acetone to give white powder of fentanyl hydrochloride. The salt was treated with 20% NaOH to give fentanyl which was recrystallised from petroleum ether (60–80°)

Yield: 13.44 g (40 %)
m.p. 82–83 °C.

Literature
The paper on synthesis of fentanyl in this manner can be found here.

mp_correction

 

[testint]

correction

View attachment 38041

Joker_55555That paper is a great read scihub was/ a godsend