# Mephedrone synthesis (4-MMC) in NMP solvent. Large scale.



## William Dampier (Sep 14, 2021)

*Reaction scheme:*
*


*​
*Reagents:*

2-Bromo-4'-methylpropiophenone (cas 1451-82-7) - 5 kg;
n-Methyl-2-pyrrolidone (NMP; cas 872-50-4) - 20 L;
Methyl amine 40% aq. solution (cas 74-89-5) - 8 L;
Benzene - 20 L;
Acetone - 30 L;
Hydrochloric acid con. aq. solution (HCl 36%) ~ 1.5 L;
Distilled water - 20 L;
Magnesium sulphate (MgSO4);

*Equipment and* *glassware**:*

100 L Batch reactor, which is equipped with drip funnel, top stirrer, thermometer, temperature control system (cooling) and reflux condenser;
Funnel;
pH indicator papers;
Several buckets 25 L;
Barrel 100 L;
Beaker 2000 mL;
Vacuum source;
Scale;
Measuring cylinder 1000 mL;
Glass rod and spatula;
Scoops;
Nutsche filter;
Rotary evaporator;












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Mephedrone hydrobromide synthesis



__ Novator
__ Aug 17, 2022
__ 5
__
2-bromo-4'-methylpropiophenone
4-mmc
bromoketone
cas 1451-82-7
meph
mephedrone
mephedrone hydrobromide
mephedrone hydrochloride
n-methylpyrrolidone
nmp




Mephedrone hydrobromide synthesis from 2-bromo-4'-methylpropiophenone with n-methylpyrrolidone...




​*Synthesis procesures*
*1.* 2-Bromo-4'-methylpropiophenone 5 kg is poured into Batch reactor or another crude 2-Bromo-4'-methylpropiophenone amount after halogenation reactions.
*2.* n-Methyl-2-pyrrolidone 20 L is poured into the reactor. Top stirrer is turned on and the reaction mixture is heated up to 40 °С.
*3.* When temperature is reached 40 °С, methylamine 40% aq. solution 8 L is poured into the reaction mixture and stirred for 20 min.
*4.* Next, distilled cold water 20 L is poured into reaction mixture and stirred for few minutes.
*5.* Benzene 15-20 L or other suitable solvent is poured into the reactor, the mixture is stirred for few minutes.
*6.* Than, the stirrer is stopped, the mixture is divided into two layers.
*7.* The bottom aqueous layer is drained through the bottom valve of the reactor. Top layer is drained into a bucket and dried over MgSO4. Than, dry solution is poured in another bucket.
*8.* Ice acetone 20 L is added to the reaction mixture and hydrochloric acid (HCl 36%) is added dropwise with a constant stirring to reach pH 5.5-6.
*9.* The mixture is put into a freezer for 12 h.
*10.* Crystallized mephedrone hydrochloride is filtered on a Nutsche filter and air dried. The yield is *58%*.

*Note*
NMP can be replaced by DMSO, DMF, Sulfolane.


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## Hans-Dietrich

How about synthesis in DСM ?


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## BHBlueberry

Wow it looks so easy.. If I only would like meph I would play with this formula


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## dark_side_of_chemistry

In 2bromo 3 chloropriofenon synthesis is the same ?


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## dark_side_of_chemistry

has anyone tried this recipe yet? any comments or tips? does 50% of the product come out?


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## William Dampier

Badbadyl said:


> In 2bromo 3 chloropriofenon synthesis is the same ?



Badbadylyes


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## dark_side_of_chemistry

thanks . I have access to 2b3ch but liquid. i understand he is already in some solvent, right?


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## William Dampier

Badbadyl said:


> thanks . I have access to 2b3ch but liquid. i understand he is already in some solvent, right?



Badbadylrather no, this is liquid in pure form


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## dark_side_of_chemistry

OK I understand . so should I mix it one to one with dsmo?


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## William Dampier (Mar 25, 2022)

Badbadyl said:


> OK I understand . so should I mix it one to one with dsmo?



BadbadylNMP 4:1 min amount. If u have large barrel, u can add proportions, it's better for reaction.


Badbadyl said:


> what do you think to carry out this reaction in such a tank? 115l. I thought to wrap it with a heating belt and install a mechanical stirrer in advance
> 
> wrapped in such a heating mantle that you can heat the reactions up to 55 degrees


Good


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## dark_side_of_chemistry

Somehow, close the upper inlet and let the methylamine drain out so as not to burst the tank, or it is better to leave it open, install only the thermometer and the stirrer.


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## dark_side_of_chemistry

is this recipe not given the wrong methylamine value? there should be no more than 8l for hot synthesis? Should this excess of methylamine be smaller during the synthesis in nmp?


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## KHaafii

How much end product do you end up with this Synthesis approximately with this recipe. For how much does uncut/Pure mephedrone go away on the market per kg? How much profit margin is there in mephedrone. Doesn't have to be petty exactly but approximately.

I have no knowledge in the market of mephedrone on a large scale. I have read that this is also fairly in demand? I don't mean for users but people who buy this for their own reasons on larger numbers.


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## dark_side_of_chemistry (Apr 21, 2022)

one question as to the amount of methylamine used in this reaction. 8l is enough for 5kg of bk4? my calculations show that 14.8l is needed.

counting process: for 1mol of bk4 we need 5mol of methylamine. 5kg bk = 5000g. 5000g / 227g = 22mol bk4. 22 mol x 5 = 110 mol methylamine. 110mol = 3416.6g ... I did 33% times because a 40% aqueous solution never has that many percent. 10353g or 14790ml of an aqueous solution of methylamine comes out ...

*these 8l of methylamine is about three times the bk4. my calculations are with a fivefold excess ... threefold is enough?*


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## ASheSChem

William Dampier said:


> 7. The bottom aqueous layer was drained through the bottom valve of the reactor.



William Dampiernoob question; 
we need to keep the bottom layer or the one above ? :x


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## William Dampier

KHaafii said:


> How much end product do you end up with this Synthesis approximately with this recipe. For how much does uncut/Pure mephedrone go away on the market per kg? How much profit margin is there in mephedrone. Doesn't have to be petty exactly but approximately.
> 
> I have no knowledge in the market of mephedrone on a large scale. I have read that this is also fairly in demand? I don't mean for users but people who buy this for their own reasons on larger numbers.



KHaafiiThe demand and prices depend on the volume of purchases of the wholesale of raw materials and your region. This synthesis is well suited for production in large quantities (ton per month and more)


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## GaDjo

Hello
I am a beginner and want to start with this synthesis. You advise me to synthesize the precursors myself or to buy them (for example on fischersci)? I want a small production, 20g maximum


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## G.Patton

SynthMaster said:


> what NMP should do in this reaction ?



SynthMasterPolar non-protic solvent


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## GaDjo

SynthMaster said:


> Hello,
> For me it is shit not synthesis. Someone tried it ? What is the yield ? Your final product will kristalized in solution of benzene and acetone ? What next, washing it by acetone ? What form has the Cristals ... ?



SynthMasterFor crystallization, you need a final step. Put you mephedrone powder on 70% Ethanol/30% H2O (1g of mephedrone for 3ml). Boil it. Poor on crystallization dishes. Wait the evaporation of ethanol and water. You've get your meph' crystals
more water you have in your solution, more your rocks will be big
(recipe found on /d/drugmanufacture, not tested)


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## Selassi

dark_side_of_chemistry said:


> one question as to the amount of methylamine used in this reaction. 8l is enough for 5kg of bk4? my calculations show that 14.8l is needed.
> 
> counting process: for 1mol of bk4 we need 5mol of methylamine. 5kg bk = 5000g. 5000g / 227g = 22mol bk4. 22 mol x 5 = 110 mol methylamine. 110mol = 3416.6g ... I did 33% times because a 40% aqueous solution never has that many percent. 10353g or 14790ml of an aqueous solution of methylamine comes out ...
> 
> *these 8l of methylamine is about three times the bk4. my calculations are with a fivefold excess ... threefold is enough?*



dark_side_of_chemistryHow many methylamine did u end up using in the cmc-synth?


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## William Dampier (Jun 16, 2022)

Selassi said:


> How many methylamine did u end up using in the cmc-synth?



SelassiYou can use a similar quantities


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## Selassi

Okay thank you


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## Selassi

We already did a succesfull synthesis of 3cmc. The help was greatly appreciated.


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## Selassi

Here is the result of the 3cmc


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## William Dampier

If you need additional help, write.


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## Yavuz1453

sir, i want to make it at home alone. can it be made in a pot and what material should i buy please help me if you can help me saddle i would be very grateful thank you


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## Selassi

Sure u can make it small scale in a flask with magnetic stirrer.


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## Yavuz1453

Yavuz1453 said:


> sir what should i do first i am a beginner thank you



Yavuz1453


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## Lucy123

William Dampier said:


> *Reaction scheme:
> View attachment 1218
> 
> Reagents:*
> ...



William DampierHello William,
Changing 2-bromo-4-methylpropiophenone with 2 
bromo, 3-chloropropiophenone will get me 3cmc. Many thanks!


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## Selassi

Lucy123 said:


> Hello William,
> Changing 2-bromo-4-methylpropiophenone with 2
> bromo, 3-chloropropiophenone will get me 3cmc. Many thanks!



Lucy123Exactly


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## Lucy123

Selassi said:


> Exactly



SelassiThanks Selassy! I guess I should keep the same proportions for the other substances? I must admit I don't have any chemistry knowledge. 
And a other question: How should I cristalaze the final result? I really appreciate all your help!


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## Selassi

Yes u can use the same amounts and proportions.


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## KHaafii

William Dampier said:


> *Reaction scheme:
> View attachment 1218
> 
> Reagents:*
> ...



William DampierWhat step should I undergo if I still have to react the bromine with the 4-methylpropiophenone. In what quantity for this scale? I also need benzene for that, right?


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## rickyrick

Is there a substitute that can be used instead of benzene?its highly carcenogenic and volatile.if not is there a viable synth of it large scale.sodium benzonate and sodium hydroxide destillation doesnt seem viable to me for large scale.importing it only option?thanks.


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## G.Patton

KHaafii said:


> What step should I undergo if I still have to react the bromine with the 4-methylpropiophenone. In what quantity for this scale? I also need benzene for that, right?



KHaafiiBromination of 4-methylpropyophenone with bromine in methylene chloride or glacial acetic acid


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## KHaafii

What is the theoretical yield mephedrone of this synthesis scheme?


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## G.Patton

KHaafii said:


> What is the theoretical yield mephedrone of this synthesis scheme?



KHaafii40-60% Are practical yields. Theoretical is 100% =)


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## rickyrick

Can benzene be substituted with toluene?


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## KWasd

Hello, I have been testing this synthesis and have a few questions about it:

1. when adding methylamine 40% in point 3, do you add it all at once, or in small portions making sure the mixture does not exceed 60 degrees?

2. point 4 mentions cold pure water, can it be cooled with dry ice to these 3-5 degrees C?

3. point 8 mentions ice-cold acetone, can I add a large amount of dry ice to it to cool it to -30 / -50 degrees C?

4. point 9 mentions putting the whole thing in the freezer, what is the purpose of this and is it necessary?


In general, I tested this synthesis, I must admit that it works and is fabulously simple, no less I used acetone at 5-10 degrees C, making the final product blue and impossible to rinse. I think it has to do with the warm acetone, at point 8, making a dimmer or some other form of impurity. Do I understand this correctly?

I would like to ask someone in the subject to answer as to the above 4 questions. Greetings


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## G.Patton

Hi.



KWasd said:


> small portions making sure the mixture does not exceed 60 degrees?



KWasdof course this


KWasd said:


> point 4 mentions cold pure water, can it be cooled with dry ice to these 3-5 degrees C?


yes, but your water will turn to ice


KWasd said:


> point 8 mentions ice-cold acetone, can I add a large amount of dry ice to it to cool it to -30 / -50 degrees C?


Yes, but you don't need to use so cold acetone. -5-10 *C Is enough


KWasd said:


> point 9 mentions putting the whole thing in the freezer, what is the purpose of this and is it necessary?


The purpose is crystallization. Low temperature helps to form crystals of mephedrone from solution.


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## WhalterWhite (Jul 20, 2022)

What efficiency is with this recipe?


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## madmoney69

who finished this synth successfully?


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## phantomwriter

Can acetone be replaced by IPA?


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## G.Patton

phantomwriter said:


> Can acetone be replaced by IPA?



phantomwriterI think no.


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## darkblink

What equipment is used for large scale production? im currently using 1000ml glass flasks for small amounts, anything metal reacts with the solution, i was thinking of using ceramic 6.5 litre slow cooker pot, mechanical stirrer and a plug in temperature control thermostat to controll temp.


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## William Dampier

phantomwriter said:


> Can acetone be replaced by IPA?



phantomwriterYes, but in small quantities. Otherwise, you will have to evaporate alcohol.


darkblink said:


> What equipment is used for large scale production?


Large glass reactors, or equipped plastic barrels


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## darkblink

Can anyone recommend a supplier of NMP to the UK?


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## Bennychairman

can the nmp be recycled?


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## G.Patton

Bennychairman said:


> can the nmp be recycled?



BennychairmanYes, just distill it.


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## rafael1985

Selassi said:


> Here is the result of 3 cmc



SelassiAfter acidification I have water how I must crystalize this ?


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## WhalterWhite (Aug 23, 2022)

Hello. I have 100 l liquid 2bromo3chloro.. , toulen , and replace Dmso Sulfolane. I try start do 3cmc.


When doing 3cmc all the steps are the same? On the forum they write that yes but I prefer to ask. So far I have done 4mmc without salivation. I mixed 2h at 40 degrees 2b4met with methylamine and toulene. Finally, I poured water with acid, separated the layers and I dry for about a week and wash with acetone and ihad 50% efficiency of 4mmc powder. Now I would like to try your recipe.

One more question. Once, a salesman instead of toulen sold me dichloromethane. However, the mephedrone layer does not come out on top of this. Is dichloromethane useful for anything? Sorry for my English, it's poor


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## Venom2021

methylene chloride is better in my opinion at 4mmc true 2h 40 ° but with 40 ° taulen it is too small the temperature must be higher than 50%, i.e. 100g bk4 50g 4mmc + a lot of impurities because you do not clean the oil at all I see after crystallization you will have somewhere 40g maybe less efficiency I obtained 70% and 80% yield on methylene chloride


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## WhalterWhite

you're right. After crystallization, I was left with 40%. And when I tried to salt the solution with caustic soda once, I had 23% efficiency left.
As for chloromethane, at 40 ° C, two layers separated with stirring for two hours. However, after 10 minutes, the color was the same and there were no two layers. Can I also use chloromethane in 3cmc?


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## Venom2021

For 4cmc the process should be the same 3cmc I did not do After 60% crystallization, this is the minimum


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## rafael1985

With 3 cmc every step are the same but after acidification with HCl 35-37% product is liquid form.You must evaporate water but is really dirty black product.With 2 bromo 4 chloro or methylo You dont have problems like with this 2 bromo 3 chloro liquid


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## rafael1985

WhalterWhite said:


> you're right. After crystallization, I was left with 40%. And when I tried to salt the solution with caustic soda once, I had 23% efficiency left.
> As for chloromethane, at 40 ° C, two layers separated with stirring for two hours. However, after 10 minutes, the color was the same and there were no two layers. Can I also use chloromethane in 3cmc?



WhalterWhiteMaybe You put to less methylamine.
For 1 kg ketone nie much You give methylamine?


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## WhalterWhite

rafael1985 said:


> Maybe You put to less methylamine.
> For 1 kg ketone nie much You give methylamine?



rafael1985on 2b4m I give 3.5 liters of methylamine. 
P.S I can see that our language got through in the translator


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## rafael1985

Selassi said:


> Here is the result of the 3cmc



SelassiCan You tell how You make powder You put cold acetone HCl and let on freezer ?


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## WhalterWhite

rafael1985 said:


> Can You tell how You make powder You put cold acetone HCl and let on freezer ?



rafael1985I didn't give to freezer. I waited and the substance will dry out which took time. Then I rinsed with acetone and there was powder. I did according to my own recipe. Now I want to try 3cmc with a refrigerator to speed up the process


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## rafael1985

WhalterWhite said:


> I didn't give to freezer. I waited and the substance will dry out which took time. Then I rinsed with acetone and there was powder. I did according to my own recipe. Now I want to try 3cmc with a refrigerator to speed up the process



WhalterWhiteWith 3 cmc you will be have more fun


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## WhalterWhite (Aug 25, 2022)

rafael1985 said:


> With 3 cmc you will be have more fun



rafael1985


rafael1985 said:


> With 3 cmc you will be have more fun


What will be more fun with? With drying? Maybe can buy grocery dryers to speed it up?


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## rafael1985

You know here is methods with this NMP extraction with bezene maybe works good but with this simply method what You make and 90 % people everyone have problem.Try evaporate but my friend say is black gum.Later they put acetone and let in freezer


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## WhalterWhite

I will try this recipe this time for 3cmc, but Dmso will change to sulfolane
Can I replace something with dichloromethane in this recipe?


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## WhalterWhite

Sorry. Nmp change to Dmf, i have better price. And benzene to toulen.Is change to efficiency?


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## rafael1985

Friend say they same maybe is better work because is little more work from 2 bromo 3 chloro but you know this simply method is for people which have no problem to buy precursors.To buy NMP and benzene is not easy I think


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## Venom2021

benzene is carcinogenic record video of 4mmc production using nmp benzene is fun and inefficient 40% of the final product very little per 100g bk4 you need to use a 2l flask I use a 2l glass bottle and it yields 300g and 350g of the final crystal product. If you are using benzene toulen dcm xylene nmp you must use different cooking temperatures and the time is different. I do not use a flask, but an ordinary wine bottle, a bucket, a conical separator for wine, cloth for filtration and a centrifuge for drying clothes.


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## Venom2021

Cristal


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## rafael1985

Venom2021 said:


> You crystalize from water or water/alcohol



Venom2021


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## WhalterWhite

Selassi said:


> Here is the result of the 3cmc



SelassiMan beautiful crystal. How did You do that?


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## KWasd (Aug 27, 2022)

Hello everyone. All the synthesis is going well until acidification. Initially everything goes correctly, a "flour" precipitates, but with the addition of HCL 36-38% the whole mixture initially becomes red until it turns strongly blue.

Such soiled gunpowder can not be washed even with a huge amount of acetone, minimally the blue color comes off, but the final product is still strongly blue, and the yield is drastically low.

When souring, will diluting HCL with acetone, for example, in a ratio of 1:5 help? Of course, the whole thing frozen using dry ice.

The second question is, when adding methylamine, should I add it in small portions so that the temperature does not exceed 60 degrees, or can I pour it all at once and not look at the temperature? Adding all the methylamine at once won't drastically reduce the output?

Greetings


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## rafael1985

You do everything like in recipe from this post?How much methylamine You put in


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## KWasd

40g 2-bromo-4-metylopropiofenon

160ml NNP

65ml metyloamina 40% in water

120ml benzen

240ml aceton

12ml HCL


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## rafael1985

How much yield You have?


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## KWasd

Using the synthesis from this topic I am coming out with a blue powder that cannot be cleaned with acetone.... i uploaded the pictures from another synthesis that i have mastered to perfection or at least i think so


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## KWasd

In point 8, I add 20L of ice-cold acetone to the reactor and only separately add HCL 36-38% slowly until the pH drops to 5? Do I mix the HCL with 20L of acetone and only add the mixture to the reactor? 

I can't figure out why during acidification the whole thing precipitates nicely until at some point it starts turning blue.... 

I bet it is due to adding too concentrated HCL 36-38% by which I burn the product and hence the blue mess.


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## Venom2021

LIke this


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## KWasd

Final blue color yes, but the liquid was not all red as in the attached photos. Normally yellow oil, white gunpowder precipitated, over time the yellow oil began to turn blue while staining the gunpowder, which could no longer be cleaned with acetone. Ultimately, after draining, the blue powder looked like this in the last photo


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## rafael1985

This staff smartness eyes before You put HCL?


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## rafael1985

My friend have the same problem maybe not all ketone reacted


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## KWasd

I honestly have no idea, I haven't checked it. In the next few days I will try to approach this synthesis again I will check it and let you know.

In my opinion, it is the fault of acidification with concentrated undiluted HCL by which the product burns and impurities are formed. Now I will want to add ice-cold acetone at step 8, and acidify successively with a 1:5 HCL:Acetone mixture. It seems to me that this will solve the problem.

The organic phase takes on a nice orange-amber color so I would argue that it is running at least correctly.


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## rafael1985 (Aug 28, 2022)

You make synthesis 3 cmc?
You know I think this simpliest method is better than this but is my opinion


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## KWasd

4mmc forever


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## KWasd

I have a question from a different point of view. Suppose you have a completely airtight room, where fresh air is forced in on one side and a high-powered fan pulls it out of the centre of the room on the other. 

How do you deal with the filtration of the odour in the air? Do you use any purifiers, if so, what kind and with what kind of cartridge, or is it enough to give a high-capacity carbon filter with activated carbon on the exhaust as is used in cannabis cultivation. If such a filter would do the job, which activated carbon is best, CTC or ordinary carbon? 

How is the air and odours filtered in the laboratories? Regards


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## OKS1945

KWasd said:


> I have a question from a different point of view. Suppose you have a completely airtight room, where fresh air is forced in on one side and a high-powered fan pulls it out of the centre of the room on the other.
> 
> How do you deal with the filtration of the odour in the air? Do you use any purifiers, if so, what kind and with what kind of cartridge, or is it enough to give a high-capacity carbon filter with activated carbon on the exhaust as is used in cannabis cultivation. If such a filter would do the job, which activated carbon is best, CTC or ordinary carbon?
> 
> How is the air and odours filtered in the laboratories? Regards



KWasdCan you share your method for 4mmc synthesis? I think carbon filter will do the job for youl.


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## None

William Dampier said:


> If you need additional help, write.



William DampierI have a tablet containing ephedrine. Can you tell me the method of extraction and synthesis with potassium carbonate and acetic acid? Of course, I heard that it is possible to synthesize with sodium hypochlorite. Here, the access to other materials is limited.


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## G.Patton

None said:


> I have a tablet containing ephedrine. Can you tell me the method of extraction and synthesis with potassium carbonate and acetic acid? Of course, I heard that it is possible to synthesize with sodium hypochlorite. Here, the access to other materials is limited.



NoneYou can open Amphetamines section, answers are there.


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## aaronstevens

1.First of all, can you please list all of the laboratory equiptment needed for this? I saw that you used a reactor in the synthesis. Is this link below what you mean?



2. And also is a Nutsche filter required. If so, can you please give me a reliable place where I can aquire one. Is there any more equiptment apart from the ones I have listed. If so please tell me what they are and the places where I can aquire them.









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3.And in one of your comments in your post, you said you can use this to produce a ton a month. I would like to know how much would 1 production take and how much finished product will come out of the first production.

4. So if you can, please give me a list of all the laboratory equiptment, places where I can buy them. I have a lot of respect for you because of the inforamtion you have posted on this forum which has helped us with our past small-scale synthesis. All because of you and other people on this forum, there has been a BOOM in our client base recently.

Hopefully you can help me sir, and everything will go well.

Best regards,

Aaron Stevens


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## G.Patton

aaronstevens said:


> 1.First of all, can you please list all of the laboratory equiptment needed for this? I saw that you used a reactor in the synthesis. Is this link below what you mean?
> 
> 
> 
> ...



aaronstevensAs @Level1 said, you need 100l batch reactor with heating system, Nutsche filter, vacuum pump. You can figure out information about items in stock here.


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## aaronstevens

thank you for your answer and help, I have another question, is the reactor, the nutsche filter and the vacuum pump, one machine? or can it be a whole set in one machine?

Is the reactor a reactor and the rest are other elements?
Can a nutsche filter be integrated in the reactor?

From what I read and looked, nutsche filter is in vacuum pump, right?
But my point is, is it possible to buy everything in one machine?

Friend, give me answers to the following questions from yesterday:
5. Synthesis questions, points 8 and 9
a.) How much hydrochloric acid to add?
b.) Add hydrochloric acid slowly or quickly?
c.) How long to freeze for and what freeze temperature should be set?


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## aaronstevens

Are the images I have attached the appropriate equiptment for the synthesis?


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## aaronstevens

Will this lab reactor work for this synthesis?





100l Lab Use Chemical Jacketed Glass Reactor Chiller Reactor - Buy 100 Liters Chemical Jacketed Glass Reactor,Chiller Reactor,Glass Reactor Product on Alibaba.com


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## aaronstevens

Will this nutsche filter work?





Glass nutsche filters - LPP Group


Buchi nutsche filters can easily be combined with Buchi reactors for solid / liquid separation after the synthesis allowing safe processing of a wide range of solvents and acids.




www.lpp-equipment.pl


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## Bennychairman

KWasd said:


> I honestly have no idea, I haven't checked it. In the next few days I will try to approach this synthesis again I will check it and let you know.
> 
> In my opinion, it is the fault of acidification with concentrated undiluted HCL by which the product burns and impurities are formed. Now I will want to add ice-cold acetone at step 8, and acidify successively with a 1:5 HCL:Acetone mixture. It seems to me that this will solve the problem.
> 
> The organic phase takes on a nice orange-amber color so I would argue that it is running at least correctly.



KWasd
did you find out why it was blue? , i followed the sythesis with 25g of bk4 and after adding 1:1 hcl acetone to the RM at one point it kinda solidefiend for a sec , then redissolved , then turned blue and bluish poweder praticipated ,


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## Bennychairman

KWasd said:


> I honestly have no idea, I haven't checked it. In the next few days I will try to approach this synthesis again I will check it and let you know.
> 
> In my opinion, it is the fault of acidification with concentrated undiluted HCL by which the product burns and impurities are formed. Now I will want to add ice-cold acetone at step 8, and acidify successively with a 1:5 HCL:Acetone mixture. It seems to me that this will solve the problem.
> 
> The organic phase takes on a nice orange-amber color so I would argue that it is running at least correctly.



KWasd
the blue color is methylamine residue i think , i did the reaction and all went well until acidification also , then powder participated and after x<ph 7 it turned blue , but i was able to wash the powder with acetone and it became white 

maybe you didnt add enough water to dissolve the methylamine and NMP into it ? i extracted with toluene, idk sometimes it looks like in their videos it works too perfect lol , but i anded up with 12.5g from 25g bk4 , not bad at all for first try


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## Bennychairman

if you get blue product it means there is too much methylamine in your organic layer , wash it with salt water 5 times and acidification should go better


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## fuckypu

12.5g powder ??
Crystal you get 10g


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## KHaafii

KWasd said:


> 4mmc forever



KWasdHi, can you share your synthesis with 4MMC and if your blue colour problem has been solved? Was it due to concentrated HCL you used?


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## Chenzen

Hi guys, I did it like this, why my powder has no power is very weak I use of this on myself 200mg 500mg and I did the zero effect the same as everyone in the movie ?? : (I wash the powder 3 times with acetone. W get blue meph too and noe is white but no effect high


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## G.Patton

Chenzen said:


> Hi guys, I did it like this, why my powder has no power is very weak I use of this on myself 200mg 500mg and I did the zero effect the same as everyone in the movie ?? : (I wash the powder 3 times with acetone. W get blue meph too and noe is white but no effect high



ChenzenHave you controlled temperature during reaction well?



KHaafii said:


> Hi, can you share your synthesis with 4MMC and if your blue colour problem has been solved? Was it due to concentrated HCL you used?


Same question for you. Was temperature of reaction is higher than 55 deg C?


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## ChingShih

Venom2021 said:


> benzene is carcinogenic record video of 4mmc production using nmp benzene is fun and inefficient 40% of the final product very little per 100g bk4 you need to use a 2l flask I use a 2l glass bottle and it yields 300g and 350g of the final crystal product. If you are using benzene toulen dcm xylene nmp you must use different cooking temperatures and the time is different. I do not use a flask, but an ordinary wine bottle, a bucket, a conical separator for wine, cloth for filtration and a centrifuge for drying clothes.



Venom2021
Can you please write your method?
for 1kg 2-Bromo-4 Metylopropiofenon?
Or write proportions you use, you can also write in PM if you don't want to share public


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## None (Oct 6, 2022)

G.Patton said:


> You can open Amphetamines section, answers are there.



G.PattonI looked, there was no synthesis with permanganate and acetic acid.


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## Mr.Blanks00

I'm sorry I want to ask how much is the price of mephedrone in Europe for 1gram,..


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## Chenzen

For 14€ to 30€
1kg for 3500€ to 8000€


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## HEISENBERG

Chenzen said:


> For 14€ to 30€
> 1kg for 3500€ to 8000€



Chenzen
It's scary to imagine what they sell you for 14€ per gram/3500 per kg
A good quality product should cost from 30/8000


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## Chenzen

If you made 1kg for for 300€ 3500€ is good price for crystal if is a lot 4mmc in city nobody give 8000€ per kg haha


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## HEISENBERG

Yes, the cost of 1 kg can be 300 euros. But this is a cost that only takes into account the purchase of chemicals. You omit the labor you put into it, the cost of equipment and much more. If you buy 50kg at once, you can find a price of 4-5 thousand euros. If someone sells a finished product for 3.5 thousand, most likely it is a low quality product or just a scam.



Chenzen said:


> if is a lot 4mmc in city nobody give 8000€ per kg haha



ChenzenThere are very few 4mmc in all of Europe, let alone any specific cities. Mephedrone is far from the most popular drug


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## G.Patton

None said:


> I looked, there was no synthesis with permanganate and acetic acid.



NoneSorry, you are right. Can you try other methods from Ephedrine extraction from pills methods or http://bbzzzsvqcrqtki6umym6itiixfhn...s/methamphetamine-from-ephedrine-tablets.302/ ?


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## KHaafii

G.Patton said:


> Same question for you. Was temperature of reaction is higher than 55 deg C?



G.PattonI was wondering myself, that's why i asked. http://bbzzzsvqcrqtki6umym6itiixfhn...mmc-in-nmp-solvent-large-scale.231/post-12368


http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/mephedrone-synthesis-4-mmc-in-nmp-solvent-large-scale.231/post-12403


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## Hongkongchen

blue meph is formed when hydrochloric acid is added too quickly, then the freebase begins to heat up and overheating produces iso mephedrone and other impurities. Product performance and quality are falling.


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## G.Patton

KHaafii said:


> I was wondering myself, that's why i asked. http://bbzzzsvqcrqtki6umym6itiixfhn...mmc-in-nmp-solvent-large-scale.231/post-12368
> 
> 
> http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/mephedrone-synthesis-4-mmc-in-nmp-solvent-large-scale.231/post-12403



KHaafiiThe product is looks white in pictures from first link.


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## G.Patton

KWasd said:


> The second question is, when adding methylamine, should I add it in small portions so that the temperature does not exceed 60 degrees, or can I pour it all at once and not look at the temperature? Adding all the methylamine at once won't drastically reduce the output?



KWasdYou have to add methylamine in portions to avoid temperature rising higher than 55 deg C.


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## Hongkongchen

G.Patton said:


> You have to add methylamine in portions to avoid temperature rising higher than 55 deg C.



G.Pattonnot necessarily, but you can, if you put everything in, you will start stirring after 15 / min the temperature will be 38 ° C and it will not rise higher, it depends on what solvent you use


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## aaronstevens

@G.Patton

Hey guys, I'm going to need some help here. I did the reaction with 1KG of 2 bromo 4 methylpropiophenone so I divided all of the quantities of the other reagents by 5 and divided the capacity of the glassware by 5.

But after doing this synthesis that William dampier posted after scaling after the freezing step the precipitate did not form.

Does anyone know a solution to this?


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## G.Patton (Oct 9, 2022)

aaronstevens said:


> But after doing this synthesis that William dampier posted after scaling after the freezing step the precipitate did not form.



aaronstevensHave you done everything as described in video? Which pH have you reached in step 8?


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## johnny.b

In freezer must be specified temperature or this is not imported?


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## Benz88

Anyone done this with Dmso?


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## aaronstevens

Ok sir, 



G.Patton said:


> Have you done everything as described in video? Which pH have you reached in step 8?



G.Pattonwe managed to form the mixture correctly we will tell you when we have formed the final product.

But we reached a PH between 5.5 and 6.


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## G.Patton

johnny.b said:


> In freezer must be specified temperature or this is not imported?



johnny.bNot so important. Approximately -15- -17 deg C.


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## ChingShih

Is it possible to do this 4mmc reaction in stainless steel pot- kettle, without condenser for cooling?
And what are the correct temperatures if using DMF instead of N-Methyl-2-pyrrolidone (NMP)?


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## Netflix

ChingShih said:


> Is it possible to do this 4mmc reaction in stainless steel pot- kettle, without condenser for cooling?
> And what are the correct temperatures if using DMF instead of N-Methyl-2-pyrrolidone (NMP)?



ChingShihPolish guys made 4mmc with like this poot


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## KHaafii (Oct 14, 2022)

Hi, will epsom salt that i just can buy from regular stores also do the work for me? Also how much is estimated used for this scale of synthesis. Few kg or are we talking couple 100 grams only.


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## ChingShih

Common guys post some pictures of your setup and finished crystals

Maybe even post 1kg batch reactions and your ratios
Make this thread alive again


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## Netflix

KHaafii said:


> Hi, will epsom salt that i just can buy from regular stores also do the work for me? Also how much is estimated used for this scale of synthesis. Few kg or are we talking couple 100 grams only.



KHaafiithe production of a few grams and a few kg is a big difference. In my opinion, xylene or dcm is the best for pare kg production, when the entire synthesis when working with the reactor takes 12 hours. every step must be well done, best try small amounts from 100g and then try after some time more and more in a few months you will see for yourself what mistakes you make because an amateur will not do a few kg at once. this is due to various factors in order not to make a mistake because one mistake can cost a lot of time and money.


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## Netflix

Sampel what im send year ago im found in old phone form Energy control barcelona Pure 4mmc hcl 97%


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## Prima4mmc

G.Patton said:


> Have you controlled temperature during reaction well?
> 
> 
> Same question for you. Was temperature of reaction is higher than 55 deg C?



G.PattonAnd should it be higher or lower than those 55-60 degrees? Because in one place someone said that you can add all the m40 at once to the NMP and not worry about the temperature, in another place you were told to keep an eye on not exceeding 60 degrees, and you are now asking if the temperature was higher than 55 degrees.

The conclusion I draw is that we should keep an eye on the temperature when adding the m40 to be in the 55-60 range or below 55, if below 55 then cool the solution as much as possible or would such a range of 50-55 be ideal.

From a table, it appears that when synthesizing 4MMC has NMP for 55-60 degrees, within 20 minutes the reaction efficiency is 98%, but already for 15 minutes at 55-60 degrees it is 71%.

So the best thing would be to add m40 so that the temperature is constantly around 55-60 degrees , and when all the m40 is added and the temperature starts to go down then use external heating to maintain that 55-60 degrees for a round 20 min.

Is it combining well to achieve maximum efficiency for NMP?


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## G.Patton

Prima4mmc said:


> Is it combining well to achieve maximum efficiency for NMP?



Prima4mmcIt is correct


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## Prima4mmc

G.Patton said:


> It is correct



G.PattonMr. colleague sorry to mix it up but the translator does not quite translate it well.

1. when adding methylamine, should I make sure the temperature does not exceed 55 or 60 degrees?

2. unless you mean that the temperature should fluctuate between 55-60 degrees when adding methylamine?

Version 1 or 2 is correct to get maximum efficiency.

Question number 3. If the temperature starts to drop below these 55 degrees after I finish adding methylamine, and it has only been, for example, 10 minutes since I started adding methylamine, should I reheat the remaining 10 minutes with an external heat source so that the total reaction time is 20 minutes at 55-60 degrees?

Thank you very much and please answer to each of the 3 questions to avoid bad exchange of information by using non-native language.


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## G.Patton

Prima4mmc said:


> does not exceed 55 or 60 degrees?



Prima4mmcNot more 55-60 deg. This statement is correct. You *don't *need apply external heating.


Prima4mmc said:


> 2. unless you mean that the temperature should fluctuate between 55-60 degrees when adding methylamine?


no


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## Chemix-Express

When adding methylamine keep an eye on the temperature not to exceed 55 or 60 degrees? (Which option chemically speaking is more suitable giving a cleaner product / higher yield?)

Any examples of what to replace Benzene with? Toulene? DCM?


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## Charlie3

cant download the video, can someone explain why?


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## Didi

Look on youtube you have this video form there is much more easy load


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## Serega

Chemix-Express said:


> When adding methylamine keep an eye on the temperature not to exceed 55 or 60 degrees? (Which option chemically speaking is more suitable giving a cleaner product / higher yield?)
> 
> Any examples of what to replace Benzene with? Toulene? DCM?



Chemix-ExpressI get the purest product in DCM, but the main thing is not to let the solution boil, keep the temperature no higher than 36C (4-mmc turns out to be impeccably clean and snow-white). Another great option is dichloroethane. also a good result is obtained when using NMP and toluene together (3:2 ratio).


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## Chemix-Express

Serega said:


> I get the purest product in DCM, but the main thing is not to let the solution boil, keep the temperature no higher than 36C (4-mmc turns out to be impeccably clean and snow-white). Another great option is dichloroethane. also a good result is obtained when using NMP and toluene together (3:2 ratio).



SeregaI am very interested in your comment. Someone has already mentioned this here on the forum.

I plan to set the temperature rigidly at 34 degrees (half of the given range of 32-36 degrees) and the reaction time at 4h.

The person who gave this information also gave proportions for this reaction.

Namely:
- 100g bk4
- 250ml DCM
- 150ml m40

1. will these proportions of reagents be correct? 
2. i am to add 1/2 m40 at the beginning and 1/2 m40 after one hour of reaction. What is the purpose of this? I understand to tame the temperature, but what difference does it make if we do it in 1 go or spread it over two approaches?

I have already had one approach to this attempt. I added everything in the proportions as above. I heated the mixture to 20 degrees and started adding the m40. Unfortunately the temperature did not start to rise on its own. After starting the heating from outside, the temperature suddenly jumped to 40 degrees. The liquid was boiling and turning off the heating did not help. 

What I think. Heat the reaction mass to 25-30 degrees before adding the m40 and only start gradually adding the m40 so as not to exceed the mentioned 36 degrees? Is this OK? Or do I heat the whole thing up to the reaction temperature of 34 degrees and only then add the m40?

I have one more question. How do I clean the free base? 

Washing the free base twice with an equal volume of 10% sodium trisulphate solution to remove any remaining bromoketone and washing it 2 times with clean water is sufficient? Is it necessary to use something else?


Why is it that when I neutralise with hydrochloric acid in acetone to pH 6, when adding the HCL:acetone mixture to the free base it starts to turn colourful. It's terribly difficult to wash the powder to snow white afterwards.

The colours that have occurred to me are blue, green, dark red and pink.


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## Jaro12

William Dampier said:


> *Reaction scheme:*
> *View attachment 1218*​
> *Reagents:*
> 
> ...



William Dampier
I have made this method few times on low scale (10g bromo) but I have problem with yield (about 25%) and with the "power" of end product (it is not enough strong).

10g 2-bromo-4-methylpropiophenone dissolved in 40mL of NMP, heated to 40 degrees and added dropwise (very slowly to control temperature) 20mL 40% methylamine (while addition of methylamine, the mixture was cooling to not exceed 55 degrees);
Stirring (350rpm) by 20 minutes (while stirring the mixture wasn't heated - temperature has slowly dropped to about 25-30 degrees);
100mL of cold water was added and next 50mL of ethyl acetate (stirred vigorously after addition);
Organic phase was separated, washed 3 times with cold water and dried with MgSO4; cooled to about -5 degrees.
50mL of cooled (-15 degrees) acetone was added;
Acidification was done by ice-cold HCl diluted in acetone (1:5) to the pH=5,7
Freezing by 2-3 hours in -20 degrees and filtered on Büchner funnel/washed with ice-cold acetone.

My questions are:
1) does the temperature of reaction is fine? Should I cool the mixture to not exceed 55 degrees?
2) does the pH= 5,7 is fine? Should I try lower pH to improve the power and yield of end product?
3) what else could I do to improve the yield and power? What I have done improper?

Thank you for any help in this case.


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## Serega

Chemix-Express said:


> I plan to set the temperature rigidly at 34 degrees (half of the given range of 32-36 degrees) and the reaction time at 4h.



Chemix-Express1) no external heating is needed!!! when methylamine is added, the mixture heats up by itself (it does not heat up instantly, while stirring it takes about 5 minutes, and the temperature starts to rise). the main task is to prevent the temperature from rising above 36C. for this, methylamine is added in portions. you can add all the methylamine at once, but then it will be more difficult to control the temperature. 2) your proportions are correct. 3) do not use acetone at the stage of acidification - replace it with ethyl acetate (then there will be no extraneous colors). acetone with acid gives an aldonic condensation reaction - hence the different colors and dirt. 4) the free base does not require further purification if the temperature has not risen above 36°C. it will be very clean. you only need to rinse it 2-3 times with cold water to remove the methylamine residue. thiosulfate is completely unnecessary here.


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## Didi

can you have a closed bottle and stir later when the solution can no longer heat itself then set the water bath to 35 ° c and stir the bottle from time to time for 3 hours ??


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## Serega

Didi said:


> can you have a closed bottle and stir later when the solution can no longer heat itself then set the water bath to 35 ° c and stir the bottle from time to time for 3 hours ??



Didino need to close the bottle (vessel). if the temperature is not higher than 36C, then it will not stink much. the main thing is not to let the DCM boil (boiling point 38C) - then the free base will turn out to be pure, and 4-Mmc will be very pure. By the way, about crystallization: I know all the answers, since this is my method


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## Serega

Didi said:


> can you have a closed bottle and stir later when the solution can no longer heat itself then set the water bath to 35 ° c and stir the bottle from time to time for 3 hours ??



Didiif the solution is no longer heated, and its temperature has begun to decrease, then the reaction is complete - proceed to the next stage. the average reaction time from the start of self-heating to the temperature decrease is from 2.5 to 3.5 hours (depending on the volume of initial reagents). that is, if the temperature itself began to decrease, then the reaction is over. everything is very simple


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## cockysavage

is there anything to replace acetone ?


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## Serega

cockysavage said:


> is there anything to replace acetone ?



cockysavageethyl acetate


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## PackMaN (Dec 13, 2022)

Tell me please. Have I correctly calculated the proportions of reagents and liquids in order to obtain 1-1.5 kg of 4-mmc for this synthesis. Thank you!

1) 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) - [1000g]
2) n-Methyl-2-pyrrolidone (NMP; cas 872-50-4) - [3000ml]
3) Methyl amine 40% aq. solution (cas 74-89-5) - [2000ml]
4) Benzene - [6000ml]
5) Acetone - [80000ml]
6) Hydrochloric acid con. aq. solution (HCl 36%) ~ [600ml]
7) Distilled water - [6000ml]


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## PackMaN

Sorry. ~ 700 - 800 mg


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## Chemix-Express

After reaching 40 degrees, I start adding m40 in small portions so as not to exceed 55 degrees. I keep the temperature in the range of 50-55 degrees C. With the initial batches of adding m40, the temperature immediately rises when it automatically falls down, I add another portion of m40. After about 15-20 minutes I am only halfway through the planned dose of m40, but when adding subsequent portions, the temperature no longer rises, but only flies strongly down. It looks as if after adding half of m40 and 15-20 minutes have passed since the start of adding it, the reaction has already taken place fully and each subsequent portion of m40 (only half has been added) no longer raise the temperature but only cools the solution strongly. What am I doing wrong? In the end, the performance reaches 20%, and the final product pinches the eyes and bites the nose.


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## G.Patton

Chemix-Express said:


> After reaching 40 degrees, I start adding m40 in small portions so as not to exceed 55 degrees. I keep the temperature in the range of 50-55 degrees C. With the initial batches of adding m40, the temperature immediately rises when it automatically falls down, I add another portion of m40. After about 15-20 minutes I am only halfway through the planned dose of m40, but when adding subsequent portions, the temperature no longer rises, but only flies strongly down. It looks as if after adding half of m40 and 15-20 minutes have passed since the start of adding it, the reaction has already taken place fully and each subsequent portion of m40 (only half has been added) no longer raise the temperature but only cools the solution strongly. What am I doing wrong? In the end, the performance reaches 20%, and the final product pinches the eyes and bites the nose.



Chemix-ExpressHello. Have you washed your reaction mixture by water after reaction? (step 4)


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## Chemix-Express

G.Patton said:


> Hello. Have you washed your reaction mixture by water after reaction? (step 4)



G.PattonYes, equal to the volume of water twice and once 10% sodium bicarbonate solution. I am surprised by the very low efficiency where I get about 53-55% on the crystal. It is also strange that when I add half of the m40, at the second half the reaction is no longer exothermic, and the temperature during addition only drops down.


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## G.Patton

Chemix-Express said:


> Yes, equal to the volume of water twice and once 10% sodium bicarbonate solution. I am surprised by the very low efficiency where I get about 53-55% on the crystal. It is also strange that when I add half of the m40, at the second half the reaction is no longer exothermic, and the temperature during addition only drops down.



Chemix-ExpressProbably you lose your yield somewhere. What pH do you reach after acidifying? Have you used fridge during crystallization? Important to follow all condition, described in video tutorial.


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## Chemix-Express

G.Patton said:


> Probably you lose your yield somewhere. What pH do you reach after acidifying? Have you used fridge during crystallization? Important to follow all condition, described in video tutorial.



G.PattonAcidification always leads to PH around 6. When you write about the refrigerator, you mean putting the neutralised freebase in the fridge to make the whole product fall out? Do you think so much product could have been dissolved? Is it normal that after adding half of the m40, the temperature stops rising on its own and the whole thing cools down? Thank you for your help


----------



## G.Patton

Chemix-Express said:


> Acidification always leads to PH around 6. When you write about the refrigerator, you mean putting the neutralised freebase in the fridge to make the whole product fall out? Do you think so much product could have been dissolved? Is it normal that after adding half of the m40, the temperature stops rising on its own and the whole thing cools down? Thank you for your help



Chemix-Express>>>When you write about the refrigerator, you mean putting the neutralised freebase in the fridge to make the whole product fall out?
yes, exactly
>>>Do you think so much product could have been dissolved?
I can't answer
>>>Is it normal that after adding half of the m40, the temperature stops rising on its own and the whole thing cools down?
Yes, it is okay. If you want to check conversion of reagents to 4-MMC, you can use TLC (look at Lab FAQ).


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## StarWars

I have a question, the one who recorded these videos probably saw what he was doing but what was written is not true. in the video you can't see that two solvents were used for cooking and only one was then washed with freebase with water and ethylene acetate and that's it, so where does anyone see benzene??


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## G.Patton

StarWars said:


> I have a question, the one who recorded these videos probably saw what he was doing but what was written is not true. in the video you can't see that two solvents were used for cooking and only one was then washed with freebase with water and ethylene acetate and that's it, so where does anyone see benzene??



StarWarsIn the video EA is used instead of benzene. What is a problem? Two solvents are EA and NMP.


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## little-flower

Hello"" I would like to do this reaction with toluen, but all are white like milk in the flask,,
can someone tell me if this is normal?,, I just use toluen at 24°C


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## StarWars

The resulting 2-bromo-4-methylpropiophenone in benzene is poured back into the clean flask and provides 200 ml of 40% methylamine (aqueous). Connect the reflux condenser, flask and thermometer (preferably) to the flask. Combined stirring and slightly warming the mixture (30-40 ºC). When the basal temperature, add as much as 300-400 ml (just use more). N-methylpyrrolidone from the dropping funnel (trickle), making sure the temperature does not exceed 60ºC. When adding N-methylpyrrolidone exothermic reaction, temperature can help. If the hands are too straight, it is a sign of overheating, it is recommended to slow down the mixing a bit to keep the temperature in the upper right corner). Once all the N-methylpyrrolidone has been poured in, let it mix for another 15 minutes. The entire reaction takes 15-25 minutes.
When we have pure powder bk4 then we use only NMP and methyloamine to cooking only...


----------

