Mephedrone (4-MMC) synthesis; easy to perform- high yielding

cartelloszetas

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Can made it much more faster and dont need use lab equipment. I see u made for fun if u will need made this way u need pay a lot monay for equipment.
U use also to much chemicals.
When u throw acid your powder need be white milf no like coffie. Of big scale u use too much acetone then and lost a lot of time too wash powder.
U can get 81% powder 75% crystal when u use dcm.
 
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K-Cyanide

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Brief update: The second crop yielded another 24,81g thus the total yield is at 335,57g or 85,94% on a m/m base. Bad? I am very pleased with the results.​

@tucoXxX: Taking the additional yield into account you will need 1000*500/335,57 equals to 1490g from the bromo ketone.

@w2x3f5: I respect your opinion but i disagree. The temperature cannot be too high as other routes with different solvents use higher temperatures. The RM didnt boil, i would call it a gentle reflux.
Also i doubt the duration of 2,5h is too long as there were still traces of unreacted bromoketone in the RM. And the color of the crude product appears darker than it is in fact.

A few words to the chaser of ultrapure 4-MMC. The paradox, that ultra pure substances have less desirable effects than others with some impurities is well known. This is especially true for 4-methyl methcathinone aka Mephedrone. I know what I am talking about, as I synthesized the substance via the route the official LE units all over the world are using as a testing standard (at least they did it a couple of years ago). The route uses MeHCl and Triethylamine and after the reaction an a/b extraction was conducted and then the substance was precipitated from a butanol solution with ether and recrystallized from THF. The result was an over 99% pure product, and now guess what how it worked out in terms of bioassays? Bingo! Inferior and very weak.....​
The attached pic shows the now twice washed product. I assume the effect it can produce is already lower than from the first one.

Take care folks!
 

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Richardrahl

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A few words to the chaser of ultrapure 4-MMC. The paradox, that ultra pure substances have less desirable effects than others with some impurities is well known. This is especially true for 4-methyl methcathinone aka Mephedrone. I know what I am talking about, as I synthesized the substance via the route the official LE units all over the world are using as a testing standard (at least they did it a couple of years ago). The route uses MeHCl and Triethylamine and after the reaction an a/b extraction was conducted and then the substance was precipitated from a butanol solution with ether and recrystallized from THF. The result was an over 99% pure product, and now guess what how it worked out in terms of bioassays? Bingo! Inferior and very weak.....


I too had this issue with mdma... I wonder if its the polymorphism or something else
 

K-Cyanide

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It's very strange what's going on here. You post a method and instead of a stimulating discussion, the first comment comes from an apparently confused guy who can do everything much better and faster. How he does it ?, he doesn't tell us this retard.

Then the next one shows up and wants to badmouth the method via pseudo-scientific contributions and remote analysis and thereby acquire customers for his synthesis business, shady.

And finally, Prof. Smart-ass, posts some cynical comments and provides exactly 0 constructive suggestions.

We're not in court here, I don't have to prove anything. The purity of the sample from the academic version was carried out in a professional laboratory with NMR spectra, Infrared and UV spectra, electrospray ionisation mass spectra etc.

I'll think twice about posting anything at all, so it's pointless. In the good old hive forum, a completely different style was cultivated. What a pity.
 
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Richardrahl

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K-Cyanide
We're not in court here, I don't have to prove anything. The purity of the sample from the academic version was carried out in a professional laboratory with NMR spectra, Infrared and UV spectra, electrospray ionisation mass spectra etc.

I know maps has been having huge issues with polymorphs ( I use this term loosely to mean hydrates, cocrystals, etc.) Mdma has at least 3 forms. And they only use form 1.

Boofing or putting the other forms such as water does not solve the issue.

Was Xray scans done as well?
 

Richardrahl

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. K-Cyanide

trial​
yield (%)​
purity (% peak area by HPLC)​
assay (% w/w by HPLC)​
1​
85.599.9599.64
2​
85.999.9699.40
3​
86.299.9999.77
4​
86.199.9599.76


MDMA·HCl was previously known to form one major crystal form (Form I) and at least four hydrates that incorporate 0.25–1 waters of hydration. (16) Our polymorphic screening process identified two new anhydrous crystal forms (Forms II and III) and established Form I as the most stable of the three. Form II can be reproducibly produced from a variety of alcoholic solvents, as well as in the presence of ethyl acetate and an ethereal antisolvent. Unlike Form III, which spontaneously converted to Form I after 2.5 weeks at ambient conditions, and could not be reproduced, Form II is shelf-stable, though it will convert to Form I under competitive equilibration conditions. Interestingly, both Form I and Form II reversibly convert into the known monohydrate; upon dehydration, the monohydrate formed from Form I will revert back to Form I, and the monohydrate formed from Form II will revert back to Form II. If crystallized from a concentrated aqueous solution with no form memory, the monohydrate will thermally dehydrate exclusively into Form I. X-ray powder diffraction spectra for all three forms are shown in Figure 2
 

K-Cyanide

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Congrats, so your product looks like this after the reaction time is over and before any washing/cleaning, correct? If so, we all are curious about your mysterious method to obtain a super clean product out of a reaction, which is per se not clean with a couple of side reactions. ;)
 

cartelloszetas

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I dont wash nothing i throw acid and aceton mix and get this all.u need know what u do freebase i made in 30min
 

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K-Cyanide

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Listen, you ṕolish son of a bitch, stop jerking people around here and get the fuck out, bloody idiot.:devilish::devilish::devilish:
 

Charlie3

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Can someone please explain this step. The organic layer is seperated in step 8. And in step 9 we add another 500ml into the mix?
 

K-Cyanide

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@Charlie3

I try to clarify this part of the procedure

  • The organic phase is separated and transferred to another beaker/flask. Fresh 500ml DCM is added to the other (aqueous) phase to extract the remaining freebase from the aqueous phase. This obviously results in 2 phases again, of which the organic phase is separated again and added to the freebase from the first separation. These combined organic phases are then washed with water, followed by acidification with dilute HCl.
Hope this clarified your question
 

Charlie3

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Very well explained! Thank you! Ill try this and post my results!
 

G.Patton

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The yield is 66%, not 79.59%.

500/227.1=2.201moles of 2b4p
2.201×213.7=470.5g is theoretical yield of 4-MMC
310.57×100÷470.5=66%

Thank you for your report!
 
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K-Cyanide

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@G.Patton I admit my mistake, I used the molar mass of the freebase instead of the hydrochloride. sorry folks shit happens. :poop::D
 

MMCHAMSTER

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l cant believe what l see here, lm searching this shit since 2011!!! There is not one week where l did not thought how cool it must be to get high on 4-MMC again but nobody haves it. Vendors with 5**** review shipped me something but l never got this MDMA xtc feeling with hornyness again:)

Please if you guys have some pls pls share!
 

Ortist

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So at what step an excess of methylamine is removed? How you can be sure that methylamine hcl is not in final product? Just curious
 

Goku

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u use water and soda baking and solvate then u wash all methyloamine form freebase. this all
 

thevines2

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Well if I make my 4mmc too pure and not stimulating I'd prob just go 2009-10 style and mix methylone with mephedrone got some amazing highs off that combo over years
 

Cruela83

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Do you remember how many milligrams of methylone and how many of mephedrone was that combo?
 
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