# 4-MMC (mephedrone) synthesis. Bromination in dichlormethane.



## Marvin "Popcorn" Sutton (Sep 13, 2021)

We'll consider mephedrone (4MMC) synthesis in this article. Dichloromethane (DCM) is used as a solvent. It has a low boiling point (~40 °C) and synthesis procedures take a little time.​
*Work conditions:*

Air temperature 20-24 ºC;
Relative humidity <60%;
Well-ventilated room (with air intake/exhaust hood);
Access to water and electricity;
*Main stages:*
1. Bromination;​2. Methylamination;​3. Separation/cleaning of the free base;​4. Acidification;​
*Bromination*



*1. *4'-Methylpropiophenone (cas 5337-93-9) 1000g and DCM 3000 ml is placed into a 10 l flask, stirred until a homogeneous solution is obtained.
*2.* A portion of bromine (Br2) 1000 g, 330 ml is poured into a drip funnel.​​*It is important to know:* Work with bromine takes special safety measures because the substance is very corrosive and toxic. Every surface, which has contact with bromine, will be completely spoiled. It is better to use long graduated pipette or graduated cylinder in order to measure volume of this substance. Bromination have to be carried out outside or in a well-ventilated room by reason that bromine is very volatile. The procedure isn't tricky but takes an attention. All glassware, which will be used for manipulations with bromine, must be cooled and absolutely dried.

*3. *Hydrochloric acid (HCl 36% aq) 50 mL is added into the reaction mixture. It is the catalyst of bromination reaction. A weak stirring is turned on and bromine addition is started. 
*4.* The first portion of bromine ~50 ml is added. The solution is turned brown and eventually is discolored. It means that the bromination reaction is taken place. You have to wait this moment, and not pour out all bromine in a one portion to avoid a violent exothermic reaction with a subsequent boiling off of the solution. 
*5.* Bromine is added from the drip funnel to the solution dropwise, when the first Br2 portion is discolored, in order to a smooth reaction course. If the solution begins to boil, the addition of bromine have to be stopped until the solution is cooled to 30-35 ºC.​​*It is important to know: *Hydrogen bromide is released during bromination. It is the caustic white gas (acid). It takes respiratory organs and eyes protection (full face mask) and well ventilated exhaust fumes hood.​


​*6.* It is necessary to make sure that the reaction has been completed after all the bromine has been poured in: reaction temperature is stopped to rising, the solution is stopped to discoloring. Then, the reaction mixture is stirred for 30-60 min. 

*7.* Obtained solution is washed from remaining bromine, it positively influence on the final product quality. The reaction mixture is washed with an equal volume of sodium thiosulfate (Na2S2O3) 10% solution or sodium bicarbonate (NaHCO3) 10% solution. The solutions is stirred well for 10 min, layers are clearly separated. The lower organic layer is taken for further manipulations. The top layer is disposed.

*8.* Next, the reaction mixture is washed with an equal volume of water to neutral pH. The washing procedure of the organic layer can be repeated several times, if it is necessary. The reaction 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) yield is ~1400g, which is already dissolved in DCM.​
*Methylamination*


*9.* Methylamine 40% aqueous solution is added to the solution from previous reaction. This reaction is also exothermic, so that methyl amine is added at slow rate in order to avoid the solution boiling. This influences on the reaction yield. Methylamine is taken in excess by reason that it is partially evaporated during the reaction. The average proportion is 2 ml per 1g of 2-Bromo-4'-methylpropiophenone. Methylamine 40% aqueous solution 2800 ml is added to 2-Bromo-4'-methylpropiophenone 1400 g. Methylamine is added via drip funnel in a thin flow or It is divided to 2-3 portions and poured in equal portions with a moderate stirring without splashing. 

*10.* The reaction mixture is stirred for 2 h at 40 ºC.​




​*Free base separation and purification*
*11.* After the mixture from the previous part is processed, the free base is washed and separated. The lower organic layer is separated from the upper aqueous layer. The organic layer is washed as described in *step 7 *(same procedures), the upper layer is scrapped. The organic layer washing is repeated several times until methylamine smell is disappeared.​

​
*12.* The mephedrone (4-MMC) free base DCM solution yield is ~3000 ml. If the organic layer is too small after methylamination, pour DCM 1-2 L. This will help to extract 4-MMC free base better. Then, layers are separated and an aqueous layer is disposed.

*13. *It is very important to separate the organic layer from the water. To be sure, you can put the DCM solution in the freezer, the remaining water will freeze and easy to separate. Also, you can dry your solution by anhydrous magnesium sulphate (MgSO4). If the water is left, problems with precipitation in the next step can happen during acidification.​
*Acidification*
*14.* The resulting mephedrone free base in the DСM is treated with hydrochloric acid. The best way salt production is HCl gasification. A 35-38% HCl hydrochloric acid water solution in acetone or isopropanol is also used in the ratio of 1 ml of hydrochloric acid per 10 ml of solvent (1:10).

The acid is added in small portions with a constant stirring. If the reaction mass become to thick, it is diluted with acetone. The mixture should be liquid enough in order to acidify 4-MMC free base evenly. White gas (HCl) is actively released during this procedure. Respiratory organs and eyes protection have to be used. In order to minimize the release of gas, it is recommended to cool the solution. During the acidification process, it is important to control the pH. At 5.5-6 pH, the acidification is stopped. The mixture is put into a freezer for several hours. After that, the product is filtered and dried. pH is controlled with pH indicator paper.​


Purification and crystallization instructions:





Mephedrone (4-MMC) powder purification


Introduction Mephedrone (4-MMC) synthesis reaction is carried out with production of some amount by-products. Also, some amount of unredacted precursor is left in the reaction mixture after reaction. It takes to purify a 4-MMC product with insufficient purity to reduce health risks. Manual As...




bbgate.com






https://bbgate.com//index.php?threads/crystallization-of-mefedrone-4mmc.72/


​


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## Hans-Dietrich

Bromination would be easier to do in a flask with a side neck, from which gaseous acid must enter the container with the absorber. For methylamination, you can use a HDPE canister with a tight-fitting stopper. Methylamine can be safely added in a trickle, the main thing is that the reaction mass does not start to boil. After adding all the methylamine, it is necessary to close the stopper and stir until the reaction mixture cools down. Then the synthesis can be considered complete. The emerald green color in the third picture indicates that there is too much unreacted 2-bromo-4-methilpropiophenone. In this case, it is necessary to distill the reaction mass with steam and separate the unreacted 2-bromo-4-methilpropiophenone, if this is not done, the product will acquire a color that will be difficult to wash. This will also get rid of the remaining methylamine. When laying 1.4 kg 2-bromo-4-methilpropiophenone you will not be able to simply take a glass rod and stir the acid in the base. A top drive agitator or similar device must be used. It is desirable to cool the reaction mass. A separatory funnel can then be used to supply the acid.


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## Hans-Dietrich

There is no doubt that this is a real synthesis )) I just expressed my comments on the process based on my experience. Welcome )))


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## Marvin "Popcorn" Sutton (Dec 4, 2021)

Thank you for your comment, your additions are very important. I'm glad that there are interested persons who contribute to the topic.
This synthesis is described directly by the chemist who performed it, I communicated with him online during the whole process and recorded. This is a first-person report of how everything happened in the lab.
This is one of the many syntheses the two of us have put together. It is a classic technique that has been worked out many times with different solvents.
For a 10L flask, this is the perfect calculated reagents charge. It is better not to distill the free base, but just to warm it at a boiling point solvent (watch the boiling point of the solvent in which the reaction takes place), although there may be different opinions here. Acidification was done in a PP bucket, adding acid from a chemical cup, and stirred with a Teflon stirrer attached to a electric screwdriver.
This is 100% real synthesis, which was carried out by me including))))


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## Hans-Dietrich (Dec 4, 2021)

Distilling the reaction mass with steam and distilling the freebase are two different processes. For steam distillation, additional water or steam is used. It looks like this: Water is added to the flask with the reaction mixture, about half of the volume of the reaction mixture and brought to a boil. The steam takes particles of the reaction mass with it and carries a receiver into the flask. The unreacted ketone will be transferred to the vapor receiver first. Green particles will be visible in the condenser. At some point, the freebase will go with steam. Then you need to change the receiver or stop the process altogether and start the salt release. Water will need to be added as it evaporates. By the way, the resulting ketone can be reused ))) You do not need to distill the entire content of the source. Something in the flask must come off. There it will be seen when the process needs to be completed. By the way, I also mixed the substance with a screwdriver and a Teflon stirrer. The screwdriver eventually burned out )))


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## Marvin "Popcorn" Sutton (Dec 6, 2021)

I decided that distilling halogen ketone with water vapor is not the end of the matter. Thanks for the explanation. But I still do it differently, I just heat the reaction mixture at the level of boiling solvent. Some of the solvent escapes with the remaining ketone and methylamine, the reaction mixture changes color and smell(DANGER! Do not inhale!).
Especially useful for those who make large volumes, so as not to look for bulky containers, you can do with enameled buckets and an electric stove and pick up the desired level of heating. But it is necessary to observe safety precautions and to carry out this procedure under a good hood or in the open air.
In order not to break the electric mixer, you need to keep the mixture liquid enough, adding acetone when it thickens. It is not necessary to acidify the entire volume, you can do it in portions.


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## Hans-Dietrich

Yes, there is logic in your words. Is that making large syntheses in a buckets is not entirely professional )). I think if the drug chemist has grown up to the production of industrial batches of the substance, then the equipment must correspond to the level ))) 

And I almost forgot ... When the reaction mixture boils after synthesis, the solvent will partially fly away, yes, and completely fly away methylamine, and the color will change unconditionally, but the ketone will not go anywhere. In any case, something more serious than banal evaporation must be done. Alternatively, add IPA and evaporate the reaction mixture 1-2 times. Maybe something else ...


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## MadHatter

I'm sorry ... which article? Do I miss something?


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## Marvin "Popcorn" Sutton (Jan 4, 2022)

You didn't miss anything, it's just beginning


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## rickyrick

What is in your opinion best bromine synthesis method?(cost effective,medium scale)


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## Hans-Dietrich

There is no better thing. There is more or less smelly.


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## rickyrick

Hans-Dietrich said:


> There is no better thing. There is more or less smelly.



Hans-Dietrichthought so.thanks.


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## MadHatter

Marvin «Popcorn» Sutton said:


> You didn't miss anything, it's just beginning)



Marvin «Popcorn» Sutton
Ah ok. Then I'll just patiently wait foor the good stuff


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## hlebsladky2

Marvin Popcorn Sutton said:


> In this article, we will look at one of the options for the synthesis of mephedrone (4MMC). We will use dichloromethane (DCM) as the solvent. It has a low boiling point and the whole synthesis goes quickly.
> 
> Conditions for the work:
> Air temperature 20-24ºC
> ...



Marvin Popcorn SuttonHello! How will adding DCM during methylamination help the freebase extract from the water? btw will it even work if bromination was done in a different way(peroxide, hydrobromide acid) ?


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## Marvin "Popcorn" Sutton

DCM does not need to be added during methylamination. It is used during bromination as a solvent for 4-methylpropiophenone. Then it also dissolves the resulting brominated bromo ketone. And at the end of the methylamination, it is the extractor of the mephedrone base. If a lot of DCM evaporates during the reactions and the free base does not form an organic layer after the methylamination, a portion of DCM is added to extract the free base.


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## Venom2021

you can see that an error has been made, the flask should be closed immediately after adding methylamine so that the gas does not escape and the solution does not overheat immediately. The color of the mephedrone freebase should be amber or yellow like morning urine. Here is red, this phenomenon is well known to me, so here we get a small quantity of 4mmc and very poor quality. This synthesis can be done in a water bath in a jar or vodka bottle. Pour methylamine all at once and mix it for 10 minutes until the solution starts to heat up to 35 ° then put the bottle in the water bath and shake the bottle every 10 minutes vigorously for 30 seconds and so for 2 hours every 10 minutes each time, thank you


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## rafael1985

How much you put HCl for one kg ketone or You only check with pH papers


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## Venom2021

On 1kg bk4 you use about 550ml to 600ml acid 37%


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## rafael1985

Ok but how is with 2 bromo 3 chloro one liter is 1,5 kg is the same for 1 kg like for 2 bromo 4 methylo?


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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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## Dxrk (Sep 4, 2022)

Hello guys. Can you guys please give a list of reagents with proportions and a list of necessary equipment. Thanks.


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## CristalKing

Venom2021 said:


> On 1kg bk4 you use about 550ml to 600ml acid 37%



Venom2021Much too much. Maximum 0,430 ml 37% HCL, better even 0,415 ml of 37% of HCL, cristals will be more transparent ...


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## kinshasa99

Marvin Popcorn Sutton said:


> In this article, we will look at one of the options for the synthesis of mephedrone (4MMC). We will use dichloromethane (DCM) as the solvent. It has a low boiling point and the whole synthesis goes quickly.
> 
> Conditions for the work:
> Air temperature 20-24ºC
> ...



Marvin Popcorn SuttonHello everyone,i have missed to stay in 5.5ph level.by mistake i adeed more hcl and the ph now is 2.can someone tell how to rise the ph.
thanks im advance.


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## kinshasa99

conect said:


> If you have more freebase 4mmc give to your solution 200ml and your ph will be higher



conectGive what bro?


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## CristalKing

kinshasa99 said:


> Hello everyone,i have missed to stay in 5.5ph level.by mistake i adeed more hcl and the ph now is 2.can someone tell how to rise the ph.
> thanks im advance.



kinshasa99In my opinion ph2-3 is perfect. Product has a little to much acid but product will be more white, If ph will be about 5-6 product could be more brown.


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## CristalKing

CristalKing said:


> Much too much. Maximum 0,430 ml 37% HCL, better even 0,415 ml of 37% of HCL, cristals will be more transparent ...



CristalKingSorry, I mean 430 g, not ml


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## kinshasa99

Venom2021 said:


> you can see that an error has been made, the flask should be closed immediately after adding methylamine so that the gas does not escape and the solution does not overheat immediately. The color of the mephedrone freebase should be amber or yellow like morning urine. Here is red, this phenomenon is well known to me, so here we get a small quantity of 4mmc and very poor quality. This synthesis can be done in a water bath in a jar or vodka bottle. Pour methylamine all at once and mix it for 10 minutes until the solution starts to heat up to 35 ° then put the bottle in the water bath and shake the bottle every 10 minutes vigorously for 30 seconds and so for 2 hours every 10 minutes each time, thank you



Venom2021So if i understand well,no need for a heating plate if you use DCM?You need only to put 2br4m ,dcm and methyl in a bottle and shake it every 10 mimutes and the bottle must stay in a water bath?sound very interesting...
Ho do you control the temperature?


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## hazel

In water he control temperature


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## kinshasa99

hazel said:


> In water he control temperature



hazel
there is no presure in the botle if is closed for 2h?


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## G.Patton

Level1 said:


> To właśnie dostaję z chińskiego 2-bromo-4-metylopropiofenonu
> -
> 2-bromo-4-metylopropiofenon
> Dcm
> ...



Level1Hello, please, translate you message to English and respect our *rules*. You can't use any language except for in common public section of BB forum. You can use your language in your country local group or in PM. Further messages on different language will be deleted.


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## Netflix

This what im use to made 4mmc


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## Netflix

4mmc hcl


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## Netflix

Drop acid and check ph tomorrow more picture


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## Netflix

4 mmc hcl in acetonie


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## breathing.fire

Somebody try make old method when for 1 kg 2b4m You give only 750 methyalmine in water 40% ?I know o e guy he give only this portion methylamine and reaction work normal with good yield.Why people give 2 l methylamine or more


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## Netflix

breathing.fire said:


> Ktoś spróbuje zrobić starą metodę jak na 1 kg 2b4m dajesz tylko 750 metyloaminy w wodzie 40% ?Znam koleś daje tylko taką porcję metyloaminy i reakcja przebiega normalnie z dobrą wydajnością.Dlaczego ludzie dają 2 l metyloaminy lub więcej



breathing.fireHow clean is the mmc bro then it is a chemist you didn't make ReplyReport •••


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## epson

Hans-Dietrich said:


> Bromination would be easier to do in a flask with a side neck, from which gaseous acid must enter the container with the absorber. For methylamination, you can use a HDPE canister with a tight-fitting stopper. Methylamine can be safely added in a trickle, the main thing is that the reaction mass does not start to boil. After adding all the methylamine, it is necessary to close the stopper and stir until the reaction mixture cools down. Then the synthesis can be considered complete. The emerald green color in the third picture indicates that there is too much unreacted 2-bromo-4-methilpropiophenone. In this case, it is necessary to distill the reaction mass with steam and separate the unreacted 2-bromo-4-methilpropiophenone, if this is not done, the product will acquire a color that will be difficult to wash. This will also get rid of the remaining methylamine. When laying 1.4 kg 2-bromo-4-methilpropiophenone you will not be able to simply take a glass rod and stir the acid in the base. A top drive agitator or similar device must be used. It is desirable to cool the reaction mass. A separatory funnel can then be used to supply the acid.



Hans-DietrichWon't the dcm dissolve the HDPE?


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## Netflix

epson said:


> Won't the dcm dissolve the HDPE?



epsonNo


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## subzero013

Marvin Popcorn Sutton said:


> We'll consider mephedrone (4MMC) synthesis in this article. Dichloromethane (DCM) is used as a solvent. It has a low boiling point (~40 °C) and synthesis procedures take a little time.​
> *Work conditions:*
> 
> Air temperature 20-24 ºC;
> ...



Marvin Popcorn SuttonHello, you could not tell me regarding one moment in the synthesis. I spend sourness under the water layer, to the free base in the DCM I add water and hydrochloric acid, then I separate the water layer with the hydrochloride of Mephedron dissolved in it and work with it further. The water layer with hydrochloride dissolved in it is transparent, but has a yellow tint and has an smell of acid, even after 3 multiple of the DCM. How can such an aqueous solution be cleaned? The smell of acid appears due to an excess of HCL, this is obvious, you can fight this amount of acid, but how to remove the yellow color? Acid alkaline extraction? If it can be used in this case, then tell me the proportion and which alkali is better to use?


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## G.Patton

subzero013 said:


> I spend sourness under the water layer



subzero013Hello, sorry, I don't understand you. You can push "Reply" on quotation and ask clearly. 


subzero013 said:


> How can such an aqueous solution be cleaned?


You can add NaHCO3 no get 6-6.5 pH

If you want to make A/B extraction, you can use any alkali (NaOH or KOH).


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## subzero013 (Nov 3, 2022)

G.Patton said:


> Hello, sorry, I don't understand you. You can push "Reply" on quotation and ask clearly.



G.Pattonto the free base in dichloromethane, I pour water at the rate of 1 liter of water per 1 kg of BK4, then add hydrochloric acid. as a result, I get water with 4 mm dissolved in it.


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## subzero013

G.Patton said:


> You can add NaHCO3 no get 6-6.5 pH
> 
> If you want to make A/B extraction, you can use any alkali (NaOH or KOH).



G.PattonOn other forums where 4mmc synthesis is discussed, it is believed that acid-base extraction contributes to the appearance of iso-4mmc and pirazins, I would like to know your opinion regarding this statement. If all the same make a full-fledged acid-base extraction, how many KOH do 1kg 4mms need? Or navigate the level of pH? To what value to alkali the solution?


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## ChemDamn

subzero013 said:


> On other forums where 4mmc synthesis is discussed, it is believed that acid-base extraction contributes to the appearance of iso-4mmc and pirazins, I would like to know your opinion regarding this statement. If all the same make a full-fledged acid-base extraction, how many KOH do 1kg 4mms need? Or navigate the level of pH? To what value to alkali the solution?



subzero013do not do that!!! acid-green extraction is not for 4-mmc. The 4-mmc free base is too brittle for this and easily decomposes during this procedure. just boil the water. hydrochloric acid (HCl) is a gas. the solvent (water) will leave - HCl will also leave. the 4-mmc resulting from the evaporation of water will need to be crushed and rinsed with acetone. but be careful!!! when there is little water left, reduce the temperature to 50C. since 4-mmc decomposes outside the solvent at temperatures >55°C.


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## ChemDamn

By the way, a useful fact. It is believed that 4-mmc decomposes at >55°C. but it is not so. when heated, 4-mmc decomposes from contact with oxygen and carbon dioxide. however, in an argon environment or nitrogen, 4-mmc does not decompose even at 300C, and a 4-mmc melt can be obtained. by the way, molten 4-mmc turns into a glassy homogeneous crystal like methamfetamine in the TV series Breaking Bad. I have personally tried it. but at home it is very difficult to provide an argon atmosphere


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## subzero013

ChemDamn said:


> do not do that!!! acid-green extraction is not for 4-mmc. The 4-mmc free base is too brittle for this and easily decomposes during this procedure. just boil the water. hydrochloric acid (HCl) is a gas. the solvent (water) will leave - HCl will also leave. the 4-mmc resulting from the evaporation of water will need to be crushed and rinsed with acetone. but be careful!!! when there is little water left, reduce the temperature to 50C. since 4-mmc decomposes outside the solvent at temperatures >55°C.



ChemDamnSo I was also afraid to conduct acid-base extraction. I have always done so, but this is a difficult task of more than 1 kg. I want to try to drive away the water to a concentration of 1 kg 4mmс per 1000 - 800 ml of water, add the reprimand (acetone or isopropanol) and send it to the freezer to precipitate the product. Before that, I would like to clean the solution well so as not to carry out repeated transistallization.


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## wannabeechemist

You can try steam distillation of resulting base. not for the whole volume if you don't want to. unreacted bromoketone will condense and you ll see green color on condenser. Leftover methlamine as well. Stop whenever you feel like you cleaned product enough. Wash with some NaHCO3 or Na2S2O3 10% solution, put in freezer to freeze any remaining water, decant the cleaned liquid add MgSO4, filter. Make salt


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## ChemDamn

subzero013 said:


> So I was also afraid to conduct acid-base extraction. I have always done so, but this is a difficult task of more than 1 kg. I want to try to drive away the water to a concentration of 1 kg 4mmс per 1000 - 800 ml of water, add the reprimand (acetone or isopropanol) and send it to the freezer to precipitate the product. Before that, I would like to clean the solution well so as not to carry out repeated transistallization.



subzero013this is the best option! this is how I usually pull out the remaining 4-mmc from the mother liquor after crystallization. solution is very dirty. I evaporate it at a boiling point (~ 100C), when a film appears on the surface of the solution, I remove it from heating. I cool it to ~ 50C and fill it with a double volume of acetone. mix well and put in the freezer for 10-15 hours. then I filter and get a very clean 4-mmc.


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## subzero013

ChemDamn said:


> this is the best option! this is how I usually pull out the remaining 4-mmc from the mother liquor after crystallization. solution is very dirty. I evaporate it at a boiling point (~ 100C), when a film appears on the surface of the solution, I remove it from heating. I cool it to ~ 50C and fill it with a double volume of acetone. mix well and put in the freezer for 10-15 hours. then I filter and get a very clean 4-mmc.



ChemDamnI thought to try the NMP as a solvent, judging by the video that are posted on this forum, the free base is cleaner than on dichlormethane, on other forums they wrote that Orto Xilole is obtained a cleaner base. Have you encountered NMP? I can’t find information about the correction of the temperature regime, it seems like it is necessary to keep 60 degrees, the video does not show that the mixture is cooling, but it can heat up much higher than 60 degrees.


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## G.Patton

ChemDamn said:


> it is very difficult to provide an argon atmosphere



ChemDamnHave you seen my post about Inert atmosphere synthesis? Nitrogen gas is quite easy to handle.


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## ChemDamn

subzero013 said:


> I thought to try the NMP as a solvent, judging by the video that are posted on this forum, the free base is cleaner than on dichlormethane, on other forums they wrote that Orto Xilole is obtained a cleaner base. Have you encountered NMP? I can’t find information about the correction of the temperature regime, it seems like it is necessary to keep 60 degrees, the video does not show that the mixture is cooling, but it can heat up much higher than 60 degrees.



subzero013Synthesis in DCM gives a very pure product if not brought to a boil (boiling DCM with water leads to hydrolysis and contamination). With NMP, everything is simple, temperature control is not needed. after the addition of methylamine, the temperature rises, reaches a plateau, and then the temperature drops. if the temperature began to decrease, then the reaction is complete. everything is simple. it usually takes about 15-20 minutes. but then you need to extract the free base from the NMP. for this I recommend using toluene or orthoxylene. for every 1kg of 4-bm, take 2.5 liters of toluene and pour 3 liters of water, stir well and the layers will separate. pick up the top layer and work with it. discard the bottom layer


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## ChemDamn

G.Patton said:


> Have you seen my post about Inert atmosphere synthesis? Nitrogen gas is quite easy to handle.



G.PattonThanks!!! great post!!! I will experiment


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## subzero013

ChemDamn said:


> Synthesis in DCM gives a very pure product if not brought to a boil (boiling DCM with water leads to hydrolysis and contamination). With NMP, everything is simple, temperature control is not needed. after the addition of methylamine, the temperature rises, reaches a plateau, and then the temperature drops. if the temperature began to decrease, then the reaction is complete. everything is simple. it usually takes about 15-20 minutes. but then you need to extract the free base from the NMP. for this I recommend using toluene or orthoxylene. for every 1kg of 4-bm, take 2.5 liters of toluene and pour 3 liters of water, stir well and the layers will separate. pick up the top layer and work with it. discard the bottom layer



ChemDamnWhat is the point of doing in Dichlormetan then? Stability of the resulting product? The boiling temperature again depends on the concentration, in a saturated solution, a certain section of time will be difficult to catch the condition on the verge of the beginning of a boil. Honestly, this is the first time I hear about the hydrolysis of dichlormethan when boiling with water. Since the NMP is so simple, why complicate the process?) In a gasoline or ortho xille, it is easier to keep the desired temperature, in time in the dichlormethan for 4 hours, that in the gasoline, in some cases, even faster in the benzene.


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## ChemDamn

subzero013 said:


> What is the point of doing in Dichlormetan then? Stability of the resulting product? The boiling temperature again depends on the concentration, in a saturated solution, a certain section of time will be difficult to catch the condition on the verge of the beginning of a boil. Honestly, this is the first time I hear about the hydrolysis of dichlormethan when boiling with water. Since the NMP is so simple, why complicate the process?) In a gasoline or ortho xille, it is easier to keep the desired temperature, in time in the dichlormethan for 4 hours, that in the gasoline, in some cases, even faster in the benzene.



subzero013the boiling point of DCM is 38.8C. you need to keep the temperature no higher than 36C, then the product will be very very clean. I could not achieve such purity in toluene, orthoxylene, benzene. I don't feel comfortable working with NMP because I don't have access to 4-bm. i make 4-bm from 4-methylpropiophenone. I use DXM as the solvent in this procedure (bromination in DXM is very convenient). but if I had 4-bm ready, then I would use NMP


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## subzero013

ChemDamn said:


> he boiling point of DCM is 38.8C. you need to keep the temperature no higher than 36C, then the product will be very very clean. I could not achieve such purity in toluene, orthoxylene, benzene. I don't feel comfortable working with NMP because I don't have access to 4-bm. i make 4-bm from 4-methylpropiophenone. I use DXM as the solvent in this procedure (bromination in DXM is very convenient). but if I had 4-bm ready, then I would use NMP



ChemDamnBut on the contrary, I get BK4 through the HBR, I thought to try the NMP, but I read a lot about the fact that the solution would be very hot, and overheating would lead to the formation of a mifedron and other undesirable impurities. In general, you have to try.


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## ChemDamn

subzero013 said:


> But on the contrary, I get BK4 through the HBR, I thought to try the NMP, but I read a lot about the fact that the solution would be very hot, and overheating would lead to the formation of a mifedron and other undesirable impurities. In general, you have to try.



subzero013in NMP, overheating is hardly possible. in addition, NMP itself is a weak base, and for this reason it prevents the isomerization of the free base 4-mmc, which is why the synthesis in NMP gives a greater purity of the reaction


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## subzero013

ChemDamn said:


> in NMP, overheating is hardly possible. in addition, NMP itself is a weak base, and for this reason it prevents the isomerization of the free base 4-mmc, which is why the synthesis in NMP gives a greater purity of the reaction



ChemDamnDoes the reaction requires heating only at the beginning, before adding methyline? Is the vacuum in the flask required during the amination? Or is everything done in an open system?


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## ChemDamn

subzero013 said:


> Does the reaction requires heating only at the beginning, before adding methyline? Is the vacuum in the flask required during the amination? Or is everything done in an open system?



subzero013the amination reaction, like any nucleophilic substitution reaction, is exothermic (it proceeds with the release of heat). heat is released by itself, that is, nothing needs to be heated. Vacuum is also not needed. the reaction vessel must be open to avoid overpressure (a stoppered vessel may burst).


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## Marvin "Popcorn" Sutton

ChemDamn said:


> the amination reaction, like any nucleophilic substitution reaction, is exothermic (it proceeds with the release of heat). heat is released by itself, that is, nothing needs to be heated. Vacuum is also not needed. the reaction vessel must be open to avoid overpressure (a stoppered vessel may burst).



ChemDamnIn most cases it is not necessary to heat the reaction mass. But if the reaction does not start or is weak, it is better to heat it up. This can be due to poor quality reagents or large amounts of water in the system. 

Synthesis in an NMP takes place without a vacuum and the reactor isn't sealed, even in an open vessel, as long as there is no splashing of the mass.


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## ChemDamn

Marvin Popcorn Sutton said:


> In most cases it is not necessary to heat the reaction mass. But if the reaction does not start or is weak, it is better to heat it up. This can be due to poor quality reagents or large amounts of water in the system.
> 
> Synthesis in an NMP takes place without a vacuum and the reactor isn't sealed, even in an open vessel, as long as there is no splashing of the mass.



Marvin Popcorn SuttonI completely agree. But I want to emphasize that for any reaction, the optimal concentration of reagents in the solvent is also important. at the right concentration, the reaction proceeds smoothly, without by-products and safely


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## Hank Schrader

Looks nice. Only ideal conditions for bromination need to be changed. The easiest way to brominate with virtually no odor is to brominate in DCM under a layer of water. Water absorbs hydrogen bromide, thus the smell and gases are practically absent in the external environment.
Thus, 50-100 liters of ketone can be brominated at a time.


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## Serega (Nov 20, 2022)

Hank Schrader said:


> Looks nice. Only ideal conditions for bromination need to be changed. The easiest way to brominate with virtually no odor is to brominate in DCM under a layer of water. Water absorbs hydrogen bromide, thus the smell and gases are practically absent in the external environment.
> Thus, 50-100 liters of ketone can be brominated at a time.



Hank SchraderUnder water +1


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## Chemix-Express

I 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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## subzero013

Chemix-Express said:


> I 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.
> 
> ...



Chemix-ExpressYou will need to cool, and not heat if you want to do at a temperature of 34 degrees. After adding methylin in 10 - 15 minutes, the mixture will begin to self -heal, heated bromketon before adding methyline. It is not particularly clear why exactly 34 degrees, dichlormethane boil with dissolved bromketon will be at high temperatures. When acidic, acetone often gives the color to Mephedron, someone recommends that it use ethylacetate instead and acidify with salt -acid isopropanol, someone to sour with water and then remove it.


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## Chemix-Express

subzero013 said:


> You will need to cool, and not heat if you want to do at a temperature of 34 degrees. After adding methylin in 10 - 15 minutes, the mixture will begin to self -heal, heated bromketon before adding methyline. It is not particularly clear why exactly 34 degrees, dichlormethane boil with dissolved bromketon will be at high temperatures. When acidic, acetone often gives the color to Mephedron, someone recommends that it use ethylacetate instead and acidify with salt -acid isopropanol, someone to sour with water and then remove it.



subzero013Hi. After reconstitution of BK4 in DCM (25-26 degrees C), the flask was placed on the agitator and the maximum stirring was turned on. Heating is disabled. The entire m40 was added at once, after 5-10 min the temperature began to rise to 35-37 degrees in 30-35 minutes, after which it began to fall down on its own. You mentioned that the whole reaction should last about 3.5-4 hours and will end when the temperature automatically begins to drop. For me, it warmed up to only 35-37 degrees in 30-35 and began to fall down. What am I doing wrong?


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## StarWars

how to calculate the amount of dcm in this synthesis??


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## G.Patton

StarWars said:


> how to calculate the amount of dcm in this synthesis??



StarWarsproportionately


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## WhalterWhite

I tried this method x ready 2b4chloro. I got cold soft rocks. After cleaning with acetone, the yield was low +- 20%.


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## WhalterWhite

This after 12 h freezer


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## Zetetic

Marvin Popcorn Sutton said:


> We'll consider mephedrone (4MMC) synthesis in this article. Dichloromethane (DCM) is used as a solvent. It has a low boiling point (~40 °C) and synthesis procedures take a little time.​
> *Work conditions:*
> 
> Air temperature 20-24 ºC;
> ...



Marvin Popcorn SuttonI greet you gentlemen! what can replace dichloromethane? available are benzene, acetone, isopropyl alcohol, ethyl acetate, petroleum ether. hope for a quick reply. five hours left and the lab will be closed.


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## StarWars

This is what im het thanks guys for help


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## Marvin "Popcorn" Sutton

Zetetic said:


> I greet you gentlemen! what can replace dichloromethane? available are benzene, acetone, isopropyl alcohol, ethyl acetate, petroleum ether. hope for a quick reply. five hours left and the lab will be closed.



ZeteticBenzene will work fine, but the methodology will change a bit. PM me and I'll tell you everything in detail.


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## Chemix-Express

Marvin "Popcorn" Sutton said:


> Benzene will work fine, but the methodology will change a bit. PM me and I'll tell you everything in detail.



Marvin &quot;Popcorn&quot; SuttonCan I also ask for some tips on the reaction to benzene? Currently, on benzene, the yield on crystal is around 53-55%. Maybe something will be useful. Regards and alletings


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## StarWars

Dont use 



Zetetic said:


> pozdrawiam Panowie! czym można zastąpić dichlorometan? dostępne są benzen, aceton, alkohol izopropylowy, octan etylu, eter naftowy. nadzieję na szybką odpowiedź. jeszcze pięć godzin i laboratorium będzie zamknięte.



ZeteticBezen is toxik use toulen or dcm


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## G.Patton

StarWars said:


> Dont use
> 
> Bezen is toxik use toulen or dcm



StarWarsIn fact, they are also toxic. With appropriate protection (well-ventilated area and face mask), any harm can be multiplied by 0.


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## breathing.fire

Anybody try do this with methylamine 33% in methanol?


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## euphoria84

I found this on a Russian forum, according to them, 100% Bromoketone reacts in 7 hours at 30 degrees Celsius


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## StarWars

Police chemist say 24h in 20°c with toulen is much synthesis best is fast pure and much.


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## euphoria84

StarWars said:


> Police chemist say 24h in 20°c with toulen is much synthesis best is fast pure and much.



StarWarswith toluene to form pyrazine


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