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

K-Cyanide

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Introduction:

In the following, forum members will be presented with a synthesis that is very easy to perform, does not take much time, and gives an exceptionally high yield. The method is a result of many years of experience and inputs from various sources that go back to the times of the legendary Hive forum. All of them deserve high recognition and a great tribute is paid to them.
Reaction:

ODP97XRsFw


Reagents:

1. 2-bromo-4'-methylpropiophenone (CAS 1451-82-7) 500 g;
2. Methylamine 40% aq – 750ml;
3. Hydrochloric acid (HCl 37%) appr. 250 ml;
4. Distilled water, clean tap water;
5. Dichloromethane 2,3l;
6. Tetrahydrofurane, (Aceton);
Procedure:

1.Dichloromethane (DCM) 1.5 l is poured into the reactor/flask and a condenser is attached.
2. 2-bromo-4'-methylpropiophenone 500 g (CAS 1451-82-7) is added.
3. The mixture is stirred until complete amount of bromoketone is dissolved.
4. Methylamine 40% aq, 750ml is added slowly with a drip funnel.
6. The mixture is stirred for 2 ½ h at 38 °C. .
XbdlI7AV6m


7 After that, the reaction is quenched by adding 7000ml ice cold clean tap water.
8. The mixture is stirred for 1-2 min and the DCM layer is separated off.
9. The remaining freebase is extracted with 500 ml DCM.
10. The combined organic layers where washed twice with 300ml water.
11. The combined washed organic layers were acidified with 2 M hydrochloric acid (37% hydrochloric acid is diluted 1:5 with water) to reach pH5.5-6 with constant stirring.
US78EsQjiw
12. The acidic extract was washed with 300 ml DCM and the water evaporated under vacuum (e.g. in a rotovap) until a viscous liquid is formed.
RI3ynuHS5l
13. After that, the mixture is poured into a buchner funnel and carefully filtered. At first only with gravity, then vacuum is applied until an off white solid is obtained.
0BdN3oh4w9

14. The crude mephedrone hydrochloride is rinsed thoroughly with cold THF (acetone if THF is not available)
3Lpl9o8gPn

15. The washed product is put into a Pyrex dish, or similar and dried to constant weight.
GrXmfbuEoa
Yield 310,57g or 79,59% of theory.
 

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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.
 

tucoXxX

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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.
cartelloszetasI would also be interested in your step-by-step procedure, mate
 

The-Hive

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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.
cartelloszetasSomebody say hive 🐝
 

tucoXxX

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I would also be interested in your step-by-step procedure, mate
 

tucoXxX

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Introduction:

In the following, forum members will be presented with a synthesis that is very easy to perform, does not take much time, and gives an exceptionally high yield. The method is a result of many years of experience and inputs from various sources that go back to the times of the legendary Hive forum. All of them deserve high recognition and a great tribute is paid to them.
Reaction:

View attachment 13954

Reagents:

1. 2-bromo-4'-methylpropiophenone (CAS 1451-82-7) 500 g;
2. Methylamine 40% aq – 750ml;
3. Hydrochloric acid (HCl 37%) appr. 250 ml;
4. Distilled water, clean tap water;
5. Dichloromethane 2,3l;
6. Tetrahydrofurane, (Aceton);
Procedure:

1.Dichloromethane (DCM) 1.5 l is poured into the reactor/flask and a condenser is attached.
2. 2-bromo-4'-methylpropiophenone 500 g (CAS 1451-82-7) is added.
3. The mixture is stirred until complete amount of bromoketone is dissolved.
4. Methylamine 40% aq, 750ml is added slowly with a drip funnel.
6. The mixture is stirred for 2 ½ h at 38 °C. .
View attachment 13947

7 After that, the reaction is quenched by adding 7000ml ice cold clean tap water.
8. The mixture is stirred for 1-2 min and the DCM layer is separated off.
9. The remaining freebase is extracted with 500 ml DCM.
10. The combined organic layers where washed twice with 300ml water.
11. The combined washed organic layers were acidified with 2 M hydrochloric acid (37% hydrochloric acid is diluted 1:5 with water) to reach pH5.5-6 with constant stirring.
12. The acidic extract was washed with 300 ml DCM and the water evaporated under vacuum (e.g. in a rotovap) until a viscous liquid is formed.
13. After that, the mixture is poured into a buchner funnel and carefully filtered. At first only with gravity, then vacuum is applied until an off white solid is obtained.
View attachment 13950
14. The crude mephedrone hydrochloride is rinsed thoroughly with cold THF (acetone if THF is not available)
View attachment 13951
15. The washed product is put into a Pyrex dish, or similar and dried to constant weight. View attachment 13953
Yield 310,57g or 79,59% of theory.
K-CyanideI want almost 1 kg of finished product. can I make it 3x the amount of reagents?
 

w2x3f5

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there is not enough solvent, 2.5 hours is too much and the temperature too high, the substance turned out to be very dirty after adding the acid.
 

SonicNL

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there is not enough solvent, 2.5 hours is too much and the temperature too high, the substance turned out to be very dirty after adding the acid.
w2x3f5The temp and time are right. You must have made a mistake.
 

w2x3f5

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The temp and time are right. You must have made a mistake.
SonicNLI see the color of his oil and there are all the errors. the temperature is high and the reaction is long, if he will make tcl during the synthesis he will see that at 35 degrees in 2 hours in dichloromethane nothing remains from 2b4m
 

Frit Buchner

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Wow you kids are buttholes. I can saw a tree down with a butter knife, but I wouldn't attack the guy using a chainsaw. The man never said he used all of the hcl, usually it is used at that point to make the Lewis acid. You add it until you reach the target ph.
 

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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w2x3f5

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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!
K-Cyanidesolvent solvent strife, the reaction rate is also different. From my own experience, I can say that with such data you have a huge admixture of various derivatives, and not only colored, but also white ...
Because of this, in the reference synthesis, the substance acts more gently, there are no pyrozine derivative impurities. Pure mmc practically does not give stimulation.
I recommend doing tcl, so you will see for yourself in this
 

DavidNichols

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solvent solvent strife, the reaction rate is also different. From my own experience, I can say that with such data you have a huge admixture of various derivatives, and not only colored, but also white ...
Because of this, in the reference synthesis, the substance acts more gently, there are no pyrozine derivative impurities. Pure mmc practically does not give stimulation.
I recommend doing tcl, so you will see for yourself in this
w2x3f5
The temperature cannot be too high as other routes with different solvents use higher temperatures
Different solvent - different tempreture range for syntesis.

Also i doubt the duration of 2,5h is too long as there were still traces of unreacted bromoketone in the RM
2,5h is unreasonably high for reductive animation in DCM with sixfold molar addition of amine. Your traces of haloketone has nothing to do with time.

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
Would you be kind and name us these nice impurities, so we can produce them instead of illegal mephedrone?

The result was an over 99% pure product
Who determined that purity and how?

now guess what how it worked out in terms of bioassays? Bingo! Inferior and very weak
Anyone who
know what I am talking
have a prescience of such a result without either bioassay or even testing.

sidereaction of this synthesis produces pyrazines, which are part of almost every red wine
Unlike ones in wine these are carcinogenic and mutagenic for a human.

The attached pic shows the now twice washed product. I assume the effect it can produce is already lower than from the first one.
Can you tell us the reason for such an assumption?
 

w2x3f5

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Different solvent - different tempreture range for syntesis.


2,5h is unreasonably high for reductive animation in DCM with sixfold molar addition of amine. Your traces of haloketone has nothing to do with time.


Would you be kind and name us these nice impurities, so we can produce them instead of illegal mephedrone?


Who determined that purity and how?


Anyone who

have a prescience of such a result without either bioassay or even testing.


Unlike ones in wine these are carcinogenic and mutagenic for a human.


Can you tell us the reason for such an assumption?
DavidNicholsThis is not my message and synthesis, you made a mistake)))))))))

And the comments are correct, I didn’t read everything, but he has a lot of impurities there.
 

Richardrahl

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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!
K-CyanideA 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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@w2x3f5 you may be right. But to be honest, who cares? I know from the product, produced with this method, that never an issue arised, even when guys injecting the stuff in large amounts. Therefore its a matter of self-responsibility how much and often people take it. ;)
 

w2x3f5

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@w2x3f5 you may be right. But to be honest, who cares? I know from the product, produced with this method, that never an issue arised, even when guys injecting the stuff in large amounts. Therefore its a matter of self-responsibility how much and often people take it. ;)
K-Cyanideon the chemical side, you have a mixture of mephedrone and pyrosine derivatives, I sent you the scheme for the formation of this impurity. the main thing is that you now know it.
 

K-Cyanide

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What are pyrosine derivatives? The scheme you sent me, deals with pyrazines and pyrazoles. I am aware that sidereaction of this synthesis produces pyrazines, which are part of almost every red wine. However, thank you for the info regarding pyrazoles which are definitely more inconvenient than pyrazines.
 

w2x3f5

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What are pyrosine derivatives? The scheme you sent me, deals with pyrazines and pyrazoles. I am aware that sidereaction of this synthesis produces pyrazines, which are part of almost every red wine. However, thank you for the info regarding pyrazoles which are definitely more inconvenient than pyrazines.
K-Cyanideit's not my native language, google doesn't translate accurately sometimes...
more important that you have impurities in the product.
 

SonicNL

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The methylamine and 2bk4 proportions are wrong. It is usually 1ml methylamine per 1g 2bk4. U might get even higher yields when adjusting this but im no expert.
 

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.
 
View previous replies…

Richardrahl

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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.
K-CyanideK-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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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.
K-Cyanide. 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
 
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