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

[Dxrk]

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

 

[CristalKing]

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 ...

 

[kinshasa99]

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
Relative humidity <60%
Well-ventilated room (with air intake/exhaust)
Access to water and electricity

Main steps:
1. Bromination
2. Methylamination
3. Separation/cleaning of the free base
4. Acidification

Spoiler: 1. BROMINATION

View attachment 904
In a 10l flask place 1000g of 4-methylpropiophenone and 3000ml of DCM, stir until a homogeneous solution is obtained.
A portion of bromine is measured in a dropping funnel: 1000g ~ 330ml.
It is important to remember: Work with bromine requires special care because the substance is very corrosive and smelly. Everything to which bromine touches cannot be recovered. It is best to dose bromine with a long graduated pipette by volume. Bromination should be done outside or in a well-ventilated room, as bromine is very volatile. The procedure is simple, but requires the utmost care. The container with bromine should be cooled with ice.
In a flask with a solution of 4-methylpropiophenone, 50 mL of hydrochloric acid is added, which is the catalyst for the bromination reaction. Turn on weak stirring and start adding bromine. The first portion of bromine is ~50ml, the solution will turn brown and will eventually discolor, this will mean that the bromination reaction has taken place. You should wait for this moment, and not pour out all the bromine at once to avoid a strong exothermic reaction, followed by boiling out of the solution. After the first portion of bromine has discolored, the bromine should be added from the funnel drop by drop, thus giving a smooth course of the reaction. If the solution begins to boil, the addition of bromine should be stopped until the solution cools to a comfortable temperature of 30-35ºC.
In the process of bromination actively released hydrogen bromide - a caustic white gas (acid), you must take care of the respiratory organs and eyes, to protect them, as well as have a good hood.
View attachment 714
After all the bromine has been poured in, it is necessary to make sure that the reaction has been completed: the temperature in the flask has stopped rising, the solution has stopped discoloring. It makes sense to hold the reaction mass for some time on stirring for 30-60 min. After completion of the reaction, the obtained solution should be washed of the remaining bromine, which will positively influence the quality of the final product. To do this, wash the reaction mixture with an equal volume of 10% sodium thiosulfate solution (or 10% sodium bicarbonate solution). Stir the solutions well in the flask for ~10min, let the layers stand clearly, select the lower organic layer for further work and dispose of the upper layer. Then wash the solution with an equal volume of water. The operation of cleaning the organic layer can be repeated several times if necessary.
The yield of this reaction is ~1400g, of bromoketone (4-methyl-alpha-bromopropiophenone) dissolved in DCM.

Spoiler: 2. METHYLAMINATION

View attachment 905
To the solution obtained in the previous reaction, we add methylamine (40% aqueous solution). This reaction is also exothermic, so methyl amine should be added at such a rate that the solution does not boil, this affects the yield. Methyl amine is taken in excess, since some of it escapes during the reaction. The average proportion is 2ml per 1g of bromoketone. We had 1400g of bromoketone, so we take 2800ml of methyl amine. To prevent the solution from boiling, add methyl amine in a thin stream from a drop funnel or divide the addition of methyl amine into 2-3 parts and pour in equal portions on moderate stirring without splashing. After all the methyl amine has been added, keep stirring for two hours at 40ºC.
View attachment 716 View attachment 715

Spoiler: 3. SEPARATION/CLEANING OF THE FREE BASE

After the mixture from the previous part is processed, we proceed to cleaning and separating the free base. First, we separate the lower organic layer from the upper aqueous layer. The organic layer goes further to work, the upper layer is scrapped. Repeat all cleaning steps as after bromination: wash the reaction mass with equal volume of 10% sodium thiosulfate solution (or 10% sodium bicarbonate solution). Stir well the solutions in the flask for ~10 min, let the layers stand clearly, select the lower organic layer for further work and dispose of the upper layer. Then rinse with an equal volume of water. The operation of cleaning the organic layer can be repeated several times until the smell of methyl amine disappears.
View attachment 771

The yield from this step is ~3000ml of DCM solution with mephedrone base (approximately equal to the volume of DCM added first to the bromination synthesis), but may be less. The DCM volatilizes well, especially if the reaction mixture was boiling hard or the layers were not separated well.
If the organic layer is too small after methylamination, it makes sense to pour 1-2L of DCM, this will help extract the free base better. And only then separate the layers and dispose of the aqueous fraction.
At this stage, 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. If the water is left behind, there may be problems with precipitation in the next step, during acidification.

Spoiler: 4. ACIDIFICATION

The resulting free base in the DСM must be treated with hydrochloric acid. The best gas to use is chlorohydrogen, which can be obtained by the effect of sulfuric acid on table salt in a gas generator. But more often a mixture of 35-38% acid (water solution) in acetone or isopropanol is used in the ratio of 1ml of hydrochloric acid per 10ml of solvent.
The acid is added in small portions, stirring the mixture constantly. If the mass begins to thicken, it is diluted with acetone. The mixture should be liquid enough for the oxidation to proceed evenly.
White gas (HCl) may be actively released during this procedure, so observe safety precautions and protect your respiratory organs and eyes. In order to minimize the release of gas, it is recommended to use cooled solutions.
During the acidification process, it is important to control the pH factor, and at a level of 5.5-6 pH, stop the acidification, and put the mixture in the freezer for several hours. After that the product is filtered and dried.
The pH-factor is controlled with indicator paper or an electronic pH meter for acids and corrosive media.

View attachment 767 View attachment 768 View attachment 769 View attachment 770
Instructions for purification and crystallization:

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/index.php?threads/purification-of-mephedrone-powder.127/

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/index.php?threads/crystallization-of-mefedrone-4mmc.72/

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.

 

[kinshasa99]

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

conectGive what bro?

 

[CristalKing]

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.

 

[CristalKing]

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

 

[kinshasa99]

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?

 

[hazel]

In water he control temperature

 

[kinshasa99]

In water he control temperature

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

 

[G.Patton]

To właśnie dostaję z chińskiego 2-bromo-4-metylopropiofenonu
-
2-bromo-4-metylopropiofenon
Dcm
Monometyloamina
Woda
do zrobienia
NaCI
Kwas HCl 35%-38%
Aceton
Ipa alkohol
kwas akrobinowy
Tego właśnie używam
Jak dobrze wyglądasz ??

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.

 

[Netflix]

This what im use to made 4mmc

 

[Netflix]

4mmc hcl

 

[Netflix]

Drop acid and check ph tomorrow more picture

 

[Netflix]

4 mmc hcl in acetonie

 

[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

 

[Netflix]

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 •••

 

[epson]

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?

 

[Netflix]

Won't the dcm dissolve the HDPE?

epsonNo

 

[subzero013]

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

View attachment 904​

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.​

View attachment 714 ​

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

View attachment 905​

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.​

View attachment 716 View attachment 715
​

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.​

View attachment 771 ​

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.​

View attachment 6846​

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/

​

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?

 

[G.Patton]

I spend sourness under the water layer

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

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).