Author Topic: pepper too MDMA via akabori and electro cell oxidation. (Read 550 times)

shroomedalice · « **on:** January 01, 2010, 03:59:13 PM »

pathway is as follows

pepper extracted continuously with IPA to give very clean piperine (I have done this many times no heat on the pepper is the key)

piperine hydrolised to pipperic acid (sedit seems to think this might not be nessacery and he may be right)

pipperic acid oxidized too piperonal (sedit proved this to work) in a manganese cell

alanine methylated to methyl alanine

akabori to mdephedrine

birch reaction useing lithium bronze but rather than the shake and bake we use ethylamine in ether so as it can be
dried properly.

I belive it should be possible to use the oxidation cell to oxidize the amino alcohol to the amino ketone methylone
instead of reducing to MDMA.

shroomedalice · « **Reply #1 on:** January 01, 2010, 04:02:07 PM »

these two posts are from WD
thankyou very much for the test

sedit
Dream Weaver
*****

Karma: +1/-0
Offline

Posts: 1761

View Profile WWW Email Personal Message (Offline)


Pepper to MDMA
« Reply #151 on: August 07, 2009, 09:53:33 AM »
   Reply with quote
Shroom, after chucking a small sample of Piperine crystals into Mn(IV) the crystals turned to gum at first and the black solution cleared up showing the oxidiser was working. After the fact(bout an hour it was checked) there was a smell simular to benzaldahyde present. Very sweet and very pleasent nothing at all like the smell of piperine but only in trace due to the small amount used(maybe 100mg or so).

Im not convinced that you even have to hydrolysis the Piperine to Piperic acid first and you may just be able to proceed straight to the oxidation to piperonal. If This indeed proved to be piperonal then a simple steam distill to recover the piperonal would make the chances of Pepper to product much more realistic by cutting the steps and losses to get to piperonal.
   Report to moderator
If you go to sleep and begin to dream that your going to sleep and having a dream.... Do you wake up?
shroomedalice
Wet Dreamer
***

Karma: +2/-0
Online

Posts: 149

View Profile WWW Email Personal Message (Online)


Re: Pepper to MDMA
« Reply #152 on: November 22, 2009, 12:00:59 AM »
   Reply with quote
nice one sedit
I have also found those refs I promised sorry for the time it took Smiley

http://www.erowid.org/archive/rhodium/chemistry/isosafrole.electro.html

http://www.erowid.org/archive/rhodium/pdf/isosafrole2piperonal.electrochem.pdf

shroomedalice · « **Reply #2 on:** January 01, 2010, 04:09:45 PM »

now for the extraction of the piperonal from the cell I belive that solvent is a must as
if we were to use steam distillation there is a chance that the low ph will destroy the md ring.

as for the akabori from what I have read (and I shall post the docs here) with methyl alanine
we should get anywere from 80% upwards as far as yeild is concerned.

there is actualy quite a lot of pipperine in pepper and so long as it is extracted with continous cold alcohol
I have found that the product comes out quite pure.

I used to use the pipperine as an insectecide so I have done the extraction many times and many ways.

soap pipperine borax and a little fly spray in alcohol will kill bed bugs and cockroches.

the borax softens there shell so the fly spray and pipperine can enter into there system and kill them.

Sedit · « **Reply #3 on:** January 01, 2010, 06:37:39 PM »

Extraction of Piperine is a breeze and recrystalization is no problem if you give the crystals time to form. Hydrolysis to piperic acid is nothing more then a NaOH reflux.

Lithium bronze can be made with ease and no stringent drying requirements of the NH₃ required. I proved this recently and it can be seen in photos over at Science madness. The Bronze formed in a test tube I was using in an attempt to dry Ammonia to see if it would condense in another flask submerged in HCl/Snow. The Ammonia never condensed but more appealing was the Bronze formed in the drying bottle. Another attempt was made and proved that rigorous drying of the Ammonia is completely unneeded and the Entrained H₂O just formed a precipitate at the bottom of the test tube more then likely lowering yeilds but posing not real issue. The bronze has a lower density then Ether and rises to the surface as a glittery liquid substance that forms small gold spheres that do not wish to join together very well. These decompose violently with the addition of R-OH to yeild the strong stench of Ammonia.

Attempting to use the bronze for anything useful on the other hand may pose a problem but thats a story for another place and time. Perhaps an attempt to reduce Toluene is in order.

If the use of Ammonia Ethylsulfate proves effective in the synthesis of Nitroethane I feel that the whole nature of using the Akabori is wasteful and unnessasary.

The use of Mn(IV) to oxidise the Piperic acid while appears effective on small scale test has not really been 100% proven yet. No isolation of piperinol has been made although there was the detection of a smell one could surely associate with an aldahyde. The test where performed on Piperine, at that and if correct then using it on piperic acid would be better and prevent a gum that formed when the Mn(IV) is added. The gum may not pose a problem though and steam distillation of the reaction mixture may recover any formed Aldahyde. I have also gone over the patents recently and found a detail that everyone seemed to over look when it came to the use of oxidising substances like Toluene to its aldahyde. The Cell needs to be run until the reaction turns Black and its at this point that the Mn(IV)persulfate is added over the course of an hour or more into warmed Toluene. This explains the low yeilds experianced when attempting to isolate anything useful from the Toluene. The smell of BnO was present but isolation proved to much to handle. In order to oxidise piperic acid an inert solvent for the acid is going to be needed. Possibly an Ether as long as we don't form peroxides which would be bad. I don't feel this will pose an issue though.

shroomedalice · « **Reply #4 on:** January 02, 2010, 09:08:37 AM »

it shouldnt be long my friend and ill be testing this shit with you.

next week I will buy my power setup (problem with buying mantles and stirrers from the states and canada)

then its just little bits and pieces unfortantly they can be costly too but hey its getting closer all the time.

im looking into a couple of other routes to X from piperonal mainly with the idea of making the reagents.

one idea is to use nitrosylsulfuric acid with methylurea to form nitrosomethylurea which will make diazomethane
in ether with out having to distill the mix (nitrosomethylurea is pritty nasty stuff I have heard though)

the other making the darzen reagent using alanine and nitrosylsulfuric acid to get us to the halide.

I would rather stir two acids and sulfur than use high temps to reduce nitrates personaly.

and I think as we have a nice patent to work off it is a lot easier to calculate the results and concentrations.

I am still a very strong beliver in that pepper to piperonal via electro cell is the way to go.

and yes for sure if we can get to nitroethane it all gets a lot easier.

though I still think akabori will have its place if the research that is going on continues as it does.

nitroethane will still require ether nitrite or if I am lucky nitrosylsulfuric acid.
akabori is a one pot then just a reduction away.

shroomedalice · « **Reply #5 on:** January 02, 2010, 12:13:28 PM »

it would appear that the idea of using nitrosylsulfuric acid in replacement of nitrite to make the halide of propionic acid from
alanine is not the easest way. here is a patent that uses just nitric and hydrochloric acid to arive at alpha chloro propionic acid in
good yeild.

from reports from other people I have spoken too the bromo version of this acid isomerises to beta bromo over time so it
may be best to use hydrochloric acid over hydrobromic. though if you were to form the ester straight away I think it would not
matter.

personaly for me darzen would be even more favourable than either nitroethane or akabori.
but probably not for every one.

SOMA · « **Reply #6 on:** January 02, 2010, 03:12:34 PM »

Just a couple of ideas:

Is sodium piperate soluble in boiling water? If so, you can add piperic acid to aqueous NaOH, CuSO4, and a tartrate or citrate to complex the CuO, and reflux for a couple of hours, after this you filter the copper oxides, rinse the filter with alcohol and you'll have an alcoholic solution of piperonal. I havent tried this, but there is a patent out there (not based in piperonal)

If you pyrolise plexyglass, or better buy the monomer, you can turn the methyl metaacrylate monomer in to methyl pyruvate in a electrolytic cell, with the MP you can make Alanine or N-Methyl alanine as you wish by the known methods of reductive amination.

At the short questions tread I tossed an idea for the making of chloropropionic from a lactate and chloroform, i'll try it as soon as I get the materials needed and a dosi-flow. The idea of the HNO3 + HCl route to a-chloro from alanine is interesting. I prefer the nitroethane methods over the a-chloro esthers, in theory you can get a 80-95% molar yield of P2P from aldehyde with the a-chloro, but with the nitroethane synths you can obtain a 80% molar yield of the P2P from the aldehyde without messing with lacrymators.

Can't both of you write detailed procedures with yields of what you have done? For example in the piperine extraction or it's degradation to piperic acid, so people can reproduce them.

shroomedalice · « **Reply #7 on:** January 02, 2010, 03:37:32 PM »

all in time for me im afraid soma.
I am still recollection my lab after a life disaster that set me nearly 5 years backwards.
but ill be back up and running in the near future and lab experaments will be back in order.
till then the only help I can be is to find papers and come up with new ideas.

probably not such a bad thing as it means I will have a much better idea of what is a worthy
experament and what is not

.

I do belive that this pepper must be cracked right open (excuse the pun)
it would make a lot of bee's very happy to be back on track with out having to worry
about keeping secrets and loosing reagents.

shroomedalice · « **Reply #8 on:** January 03, 2010, 04:28:48 AM »

lacrymators dont realy bother me all that much to be honest.

ive worked with chloro acetone and benzyl chloride and benzyl bromide.

even the oc spray the pigs have doesnt realy bother me all that much.

thats probably why I like eating raw chilli

the only time I have had a problem is when a 10L loomins went pop on me hehe that was funny as to be honest.
I remeber telling ever one to run then bang off she went.

but if you were to use lacrymators on a small scale and you had a towel wet with ethanol hung over the front of
your fume fume hood there is realy no way that you could hurt your self.

the ethanol will just suck the lacrymators out of the air and into the towel.

it will also remove a lot of the smell that these compounds create.

make sure you wash your flasks with ethanol though becouse if you use water you will be in a lot of pain.

if you read the patent you will also see that you can just add a nitrate to HCl then use this to convert alanine to
the chloro acid.

I dont think there is an easier way to be honest and every thing is very very OTC.

once you have the chloro acid its just a case of putting it in ethanol then gassing the ethanol with HCl
to make the ester.

evap ethanol off of the ester with a touch of xylene to make sure it is dry then distill to get a very pure
and dry darzen reagent.

the lactic acid is probably going to be of great use though as with all great ideas there is a group of pigs
ready to ban what ever is needed to use them.

SEDIT for a solvent I would have thought DCM would have been the go.

DCM also lends it self to continous extraction very well and it does not oxidise to my knowllage.

SOMA · « **Reply #9 on:** January 03, 2010, 01:42:27 PM »

I didn't see the nitrate part... that patent is the bomb, now it has to be tried to know if its a gem or pure BS as many other patents...

shroomedalice · « **Reply #10 on:** January 04, 2010, 06:08:06 AM »

ye its in there look at the densities of the three examples when it comes to nitric acid

then you will see just before the examples and explanation of how either nitrate and HCl will work or nitric and chloride will work.

the densities of the nitric allow you to use a lower conc of nitric so you will be able to use the HCl as a nitric generator insitu.

I know its got me all soft and gooey inside

and she is cheap as chips.

still that does not mean we dont need other ways. the key I think is for every one to get the darzen down.

just becouse we have the reagent doesnt mean we have the reaction down.

once we have the reaction and are used to the reagent we will be able to make it other ways and know if it will
work or not just by simple test before we waist our aldehyde.

I would sujest first trials to be done with benzaldehyde.

mostly I like this as it may kind of step some of the evil clowns here

away from ice which as much as WD may scream otherwise
fucks lives and families.

I love the idea of using sellenium dioxide on asarone then the persulfate cell on the 2,5 dimethoxy propenyl benzene.

once we have the aldehyde barium reports 79% yeild to ketone. damb man thats so cool for me.

sellenium is so fucking easy to get too.

poisoninthestain · « **Reply #11 on:** February 17, 2010, 04:32:34 AM »

This reminds me of a time forever ago with pepper...tried extraction of commercial food-grade black pepper once as per a lab manual from the 60's I found in the o-chem bookshelf on my campus....for shits and giggles i decided to mess around while cutting corners here and there because well...i'm a lazy bastard.

...~30g grounds were refluxed in 91% IPA for 1.5h, let cool, vac filtered starches out which weighed quite a bit, distilled off half of solution, quenched with 3 equivalents H2O to which a yellow coffee cream turbidity became apparent(piperine

), let settle for 24h, then chilled for 20min...vac filtered to obtain a greenish-yellow resin...yuck. I just threw the whole mess out. Twas a nightmare cleaning my buchner out of that gunk...should've used a dilute hydroxide/less heat somewhere in the extraction to remove that crap before i decided to fudge around

never thought it be that much resin though...

on another note, piperine is easily had commercially....oxidative cleavage of piperic acid after hydrolysis of piperine with oxone is kinda sexy sounding.

Sedit · « **Reply #12 on:** February 17, 2010, 05:52:49 AM »

Recrystalize that resin with Acetone and an Alcohol. The acetone will hold the resin in solution and allow your product to crystalize out. Use just enough alcohol to dissolve the remains after dissolving all that can be in acetone.

Author Topic: pepper too MDMA via akabori and electro cell oxidation. (Read 550 times)

shroomedalice

pepper too MDMA via akabori and electro cell oxidation.

shroomedalice

Re: shrooms idea for an MDMA synthesis :)

shroomedalice

Re: shrooms idea for an MDMA synthesis :)

Sedit

Re: pepper too MDMA via akabori and electro cell oxidation.

shroomedalice

Re: pepper too MDMA via akabori and electro cell oxidation.

shroomedalice

Re: pepper too MDMA via akabori and electro cell oxidation.

SOMA

Re: pepper too MDMA via akabori and electro cell oxidation.

shroomedalice

Re: pepper too MDMA via akabori and electro cell oxidation.

shroomedalice

Re: pepper too MDMA via akabori and electro cell oxidation.

SOMA

Re: pepper too MDMA via akabori and electro cell oxidation.

shroomedalice

Re: pepper too MDMA via akabori and electro cell oxidation.

poisoninthestain

Re: pepper too MDMA via akabori and electro cell oxidation.

Sedit

Re: pepper too MDMA via akabori and electro cell oxidation.