From Black Pepper To MDMA Theory

[T0lek511]

Hi,
This is my first big project in organic chemistry. So your help is welcome.
My theory is isolate a piperine from black pepper and convert to a piperic acid. And reaction with potassium permanganate cause a oxidative cleavage and makes piperonal and piperonylic acid (Is possible this acid convert to piperonal?)
After this steps is it normal synthesis of MDMA. Makes MDP2P and from MDP2P to MDMA.
What is your opinium about this route?

 

[archae]

Kinda OTC black pepper to MDMA synthesis​

Credit to u/CannaTFF over on Reddit

Black pepper to MDMA
https://chemistry.mdma.ch/hiveboard/methods/000321699.html black pepper to MDA
1. Black pepper piperine extraction
place 25g (1) of ground black pepper in a 500mL round-bottomed flask, add 250mL of 99% isopropanol with magnetic stirrer or boiling chips (2), and heat at reflux for 2-4h. Filter the mixture by suction filtration and then concentrate the filtrate to a volume of 10-15mL by simple distillation or by use of a rotary evaporator. to 20mL of a 10% solution of KOH/NaOH in 99% isopropanol contained in a 200ml beaker add the concentrated pepper extract. heat the resulting solution and add water dropwise. a yellow precipitate forms. add water until no more solid appears to form and then allow the mixture to stand at least overnight in a fringe 3-4 Celsius (3). collect the solid by suction filtration and recrystallize it with 20-30mL of isopropanol (4). (1) this extraction may be scaled up to twice the amounts specified without difficulty. If a Soxhlet extractor is available, this would be an apparatus superior to a standard reflux setup. (2) magnetic stirring or boiling chips are necessary to prevent serious bumping. (3) it is best to allow piperine to completely precipitate out by allowing the mixture to stand until the next laboratory period. (4) in our hands ca. 1-2g of piperine, mp 127-128°C, was collected upon recrystallization.
https://erowid.org/archive/rhodium/chemistry/3base/piperonal.pepper/piperine.pepper/index.html
100g of pepper = 4g-8g of piperine
(Recommendation) to buy piperine supplement powder from eBay or Bezos(amazon)
2. Hydrolysis of Piperine to Piperic acid
(2) Hydrolysis of Piperine to Piperic Acid: (These instructions are in the small scale, obviously they can be increased) Heat mixture of 0.1g piperine and 10ml of 2M ethanolic potassium hydroxide under reflux for 1.5h. Evaporate the ethanolic solution to dryness under vacuum. Suspend the solid potassium piperate that remains in the flask in about 5ml of hot water and carefully acidify the suspension with 6M HCL. Collect the precipitate, wash with cold water, recrystallize from COLD ethanol. The mp of the product should be around 206C (a little less than the literature values due to the slight Chavacine impurification (Chavacine is the Z, Z isomer of piperic acid (E, E))
75-85% theoretical yeild
http://www.sciencemadness.org/talk/viewthread.php?tid=4465
Oxidation of Piperic acid to piperonal
Materials5g piperic acid16.9g NaOH25.6g CuSO4* 5H2O150mL DCM205mL H2Osuff. HCl(aq) to acidifyProcedure

1. Combine piperic acid, NaOH, CuSO4 * 5H2O, and H2O.
2. Reflux for 8 hours.
3. Collect liquid via suction filtration, discarding solids.
4. Acidify with HCl(aq).
5. Extract product with 3x50mL DCM.
6. Distill extract to recover DCM, if desired.Yield: 4.5g piperonal

Nitroethane preparation
https://chemistry.mdma.ch/synthforum/about417-0-asc-0.html
https://erowid.org/archive/rhodium/chemistry/nitroethane.html
https://www.prepchem.com/synthesis-of-nitroethane/
Conversion of Piperonal to MDP2P
https://bitnest.netfirms.com/Rhodium/chemistry/mdp2np.html direct-ish to MDP2NP
Piperonal 35g = 30g of MDP2NP = 15g of MDP2P
https://erowid.org/archive/rhodium/chemistry/mdp2p.piperonal.html decent mdp2p
Piperonal 35g = 31g of 2 nitroisosafrole =21g of MDP2P (highest yield)
https://chemistry.mdma.ch/hiveboard/novel/000399715.html MDP2NP=MDP2P
Piperonal 35g = MDP2NP 37g= 18g MDP2P
MDP2P to MDMA
https://chemistry.mdma.ch/hiveboard/newbee/000531792.html
https://erowid.org/archive/rhodium/chemistry/redamin.os-bs.html




----------------------


Personal comment : You might want to use white pepper instead of black, its much cleaner. And if you want an easier way to make MDMA, you might want to look into the ethylvanillin route

 

[T0lek511]

Kinda OTC black pepper to MDMA synthesis​

Credit to u/CannaTFF over on Reddit

Black pepper to MDMA
https://chemistry.mdma.ch/hiveboard/methods/000321699.html black pepper to MDA
1. Black pepper piperine extraction
place 25g (1) of ground black pepper in a 500mL round-bottomed flask, add 250mL of 99% isopropanol with magnetic stirrer or boiling chips (2), and heat at reflux for 2-4h. Filter the mixture by suction filtration and then concentrate the filtrate to a volume of 10-15mL by simple distillation or by use of a rotary evaporator. to 20mL of a 10% solution of KOH/NaOH in 99% isopropanol contained in a 200ml beaker add the concentrated pepper extract. heat the resulting solution and add water dropwise. a yellow precipitate forms. add water until no more solid appears to form and then allow the mixture to stand at least overnight in a fringe 3-4 Celsius (3). collect the solid by suction filtration and recrystallize it with 20-30mL of isopropanol (4). (1) this extraction may be scaled up to twice the amounts specified without difficulty. If a Soxhlet extractor is available, this would be an apparatus superior to a standard reflux setup. (2) magnetic stirring or boiling chips are necessary to prevent serious bumping. (3) it is best to allow piperine to completely precipitate out by allowing the mixture to stand until the next laboratory period. (4) in our hands ca. 1-2g of piperine, mp 127-128°C, was collected upon recrystallization.
https://erowid.org/archive/rhodium/chemistry/3base/piperonal.pepper/piperine.pepper/index.html
100g of pepper = 4g-8g of piperine
(Recommendation) to buy piperine supplement powder from eBay or Bezos(amazon)
2. Hydrolysis of Piperine to Piperic acid
(2) Hydrolysis of Piperine to Piperic Acid: (These instructions are in the small scale, obviously they can be increased) Heat mixture of 0.1g piperine and 10ml of 2M ethanolic potassium hydroxide under reflux for 1.5h. Evaporate the ethanolic solution to dryness under vacuum. Suspend the solid potassium piperate that remains in the flask in about 5ml of hot water and carefully acidify the suspension with 6M HCL. Collect the precipitate, wash with cold water, recrystallize from COLD ethanol. The mp of the product should be around 206C (a little less than the literature values due to the slight Chavacine impurification (Chavacine is the Z, Z isomer of piperic acid (E, E))
75-85% theoretical yeild
http://www.sciencemadness.org/talk/viewthread.php?tid=4465
Oxidation of Piperic acid to piperonal
Materials5g piperic acid16.9g NaOH25.6g CuSO4* 5H2O150mL DCM205mL H2Osuff. HCl(aq) to acidifyProcedure

1. Combine piperic acid, NaOH, CuSO4 * 5H2O, and H2O.
2. Reflux for 8 hours.
3. Collect liquid via suction filtration, discarding solids.
4. Acidify with HCl(aq).
5. Extract product with 3x50mL DCM.
6. Distill extract to recover DCM, if desired.Yield: 4.5g piperonal

Nitroethane preparation
https://chemistry.mdma.ch/synthforum/about417-0-asc-0.html
https://erowid.org/archive/rhodium/chemistry/nitroethane.html
https://www.prepchem.com/synthesis-of-nitroethane/
Conversion of Piperonal to MDP2P
https://bitnest.netfirms.com/Rhodium/chemistry/mdp2np.html direct-ish to MDP2NP
Piperonal 35g = 30g of MDP2NP = 15g of MDP2P
https://erowid.org/archive/rhodium/chemistry/mdp2p.piperonal.html decent mdp2p
Piperonal 35g = 31g of 2 nitroisosafrole =21g of MDP2P (highest yield)
https://chemistry.mdma.ch/hiveboard/novel/000399715.html MDP2NP=MDP2P
Piperonal 35g = MDP2NP 37g= 18g MDP2P
MDP2P to MDMA
https://chemistry.mdma.ch/hiveboard/newbee/000531792.html
https://erowid.org/archive/rhodium/chemistry/redamin.os-bs.html




----------------------


Personal comment : You might want to use white pepper instead of black, its much cleaner. And if you want an easier way to make MDMA, you might want to look into the ethylvanillin route

archaeThank you very much for your help

 

[Passliem]

Thank you very much for your help

T0lek511Can you write about the results if you have tried it?

 

[UWe9o12jkied91d]

Can you write about the results if you have tried it?

PassliemI know of someone who extracted piperine and converted to piperic acid so it works up to that point at least

 

[Sneaky.Base]

Greetings. The route you mentioned a bove works but i want to ask you a question , did you do the synthesis by your own or just some theoreticals.
.Each kg black pepper gives you 40 gr piperine at best conditions.
. Second step is ok
. But the third step (oxidation of piperic acid to piperonal )
. Swim did it before ,only by kmno4 , and it didnt work. Cleavage in this reaction required strong oxidating agent like pio4. But with pio4 works but very low.
The cost of this reaction is not worth it
For 100 gr piperonal from this method you ll need :
30 lit ethanol or iso...
12 kg black pepper
1.5 kg cacl2
2 lit hcl
5 lit dcm
700 gr kmno4
800 gr potassium periodate
2.5 kg koh
700 gr magnesium sulphate
And a lot of lab work
Calculate the cost of these stuff in your city



But there are good news because ozonolysis is new way to get piperonal from piperine directly in cheaper way .
Im not saying i m the pro guy while mabye smone else did the oxidating step by only kmno4 .

 

[archae]

Greetings. The route you mentioned a bove works but i want to ask you a question , did you do the synthesis by your own or just some theoreticals.
.Each kg black pepper gives you 40 gr piperine at best conditions.
. Second step is ok
. But the third step (oxidation of piperic acid to piperonal )
. Swim did it before ,only by kmno4 , and it didnt work. Cleavage in this reaction required strong oxidating agent like pio4. But with pio4 works but very low.
The cost of this reaction is not worth it
For 100 gr piperonal from this method you ll need :
30 lit ethanol or iso...
12 kg black pepper
1.5 kg cacl2
2 lit hcl
5 lit dcm
700 gr kmno4
800 gr potassium periodate
2.5 kg koh
700 gr magnesium sulphate
And a lot of lab work
Calculate the cost of these stuff in your city



But there are good news because ozonolysis is new way to get piperonal from piperine directly in cheaper way .
Im not saying i m the pro guy while mabye smone else did the oxidating step by only kmno4 .

Sneaky.BaseThe above procedure hasn't been developed to maximize profit, but to be almost entirely OTC. Even if starting from piperine, it would be much easier and cost effective to get it commercially