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DnzLBhvNV1
Methylone (3,4-Methylenedioxymethcathinone, βk-MDMA) is a synthetic substance of the cathinone class that is often compared to MDMA. This product is very popular and causes a strong euphoria and empathy. It acts as a powerful aphrodisiac, the effect of which causes an unrestrained desire to have sex.
LvPtWE6U08
This article describes the synthesis of a small amount of methylone. I would like to note that the reaction scales linearly and the proportions of all substances are maintained. Methylone is quite easy to produce in large quantities. Its production does not require sophisticated laboratory equipment. This article describes the technology for producing methylone from halogen ketone (2-bromo-3,4-methylenedioxypropiophenone), which is obtained by standard bromination from 3,4-methylenedioxypropiophenone (3,4-(methylenedioxy)phenyl-1-propanone (MDP1P)).

Reagents:
  • 3,4-Methylenedioxypropiophenone (MDP1P; cas 28281-49-4) 20 g;
  • Dichloromethane (DСM) 90 ml;
  • Bromine (Br2) 22 g;
  • Sodium thiosulfate (Na2S2O3) aq solution 10% ~50 ml;
  • Distilled water;
  • n-Methylpyrrolidone (cas 872-50-4) 50 ml;
  • Methylamine aqueous 40% 20 ml;
  • Sodium bicarbonate 12 g;
  • Magnesium sulphate (MgSO4) ~30 g;
  • Hydrochloric acid (~35%) ~10 ml;
  • Acetone;
Equipment and glassware:
  • Flat bottom flask 250 ml;
  • Retort stand and clamp for securing apparatus (optional);
  • Magnetic stirrer;
  • Reflux condenser (optional);
  • Funnel;
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (500 mL x1, 250 mL x2; 100 mL x2);
  • Vacuum source;
  • Laboratory scale (0.1-200 g is suitable);
  • Measuring cylinders 100 mL;
  • Cold water bath;
  • Glass rod and spatula;
  • Separatory funnel 1 L (optional);
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Filter paper;
Synthesis procedures
MDP1P 20 g is dissolved in DСM 60 ml and a few drops of hydrochloric acid are added, then bromine 22 g is added dropwise. The reaction is exothermic, the reaction mixture is become dark, then become light by reason of hydrobromide (white gas) releasing. The remaining bromine is removed with 10% sodium thiosulfate aq solution and reaction mixture is washed with water after the end of this reaction. The organic layer can be used for the methylamination reaction (yield ~140% MDP1P) or distill off DСM under vacuum to a solid.

The synthesis is conducted under normal conditions. 2-Bromo-3,4-methylenedioxypropiophenone 10 g from previous step is dissolved with n-methylpyrrolidone 50 ml in the reaction flask. The mixture is stirred until solids are dissolved.
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Methylamine aqueous 40% 20 ml is added to the mixture, the flask is closed and stirred vigorously. Exothermic reaction have to be controlled. The reaction ends in 10 min and temperature decrease.

The exothermic reaction can be very violent and a forced cooling is necessary in case of large load. The flask should be immersed into a cold water bath for cooling. It is important to keep the temperature below 55 ºC.
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Methylone free base purification
The reaction mass is washed with sodium bicarbonate solution after reaction end, which is prepared in advance (water 120 ml and sodium bicarbonate 12 g). Sodium bicarbonate solution is poured into the reaction mixture and stirred vigorously for 1-2 min.
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Dichloromethane (CH2Cl2) 30 ml is added and stirred vigorously for 5 min. Methylone free base is extracted by DCM from this mixture. Organic layer is separated with help of separatory funnel.
CYFu1wPcRQ
Extraction
Layers separation in separating funnel (Photo 1). The bottom layer is DCM extract with cathinone base. The aqueous fraction is top layer, which have to be separated and extracted one more time with DCM 30 ml (Photos 2-3-4). The lower organic layers are combined and washed with distilled water 60 ml 3-4 times in separatory funnel until the methylamine smell absent (Photo 5-6). Methylone free base in DCM is always in the bottom layer. Layers are separated carefully. Try to avoid getting water into the organic layer. Organic solution is dried over MgSO4.
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Acidification
Methylone free base solution in DCM is diluted with an equal volume of dry acetone (Laboratory grade 99%+). Then hydrochloric acid (~35%) is added in small portions dropwise. The mixture is stirred constantly and pH is controlled. A precipitate is appeared. If the mixture became very thick, acetone is added.
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The mixture must be very liquid in order to acidify methylone properly. When pH is reached 5.5-6, HCl addition is stopped. The mixture is cooled and filtered.
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If methylone hydrochloride is not pure enough, you can read how to purify it here. Large crystals producing is described in this article.

Methylone hydrochloride purification with dry acetone gives a good result. There are several pictures of methylone hydrochloride before and after purification procedure.
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ELiAWq8a9r
 
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BHBlueberry

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good M1 have a great blow - for me even too great to produce it :) You use a lot of DCM here, I don't like it, can I replace it with anything else? (Ether?)
 

karamelosanto

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HI, Thanks for sharing this synthesis, I think is very clear.
I am from South America and here is a little difficult to find DCM. However, I can try to find it in some way. Maybe buying it from china.
I want to ask. Can you put all the regents in a list with quantities to make a little more easy to understand what I must to buy. If is possible with an estimated price.
Thanks!!!
 
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HI, Thanks for sharing this synthesis, I think is very clear.
I am from South America and here is a little difficult to find DCM. However, I can try to find it in some way. Maybe buying it from china.
I want to ask. Can you put all the regents in a list with quantities to make a little more easy to understand what I must to buy. If is possible with an estimated price.
Thanks!!!
karamelosantoDCM can be replaced by a more readily available solvent. The quantities of reagents depend on your needs.
I wrote to you on the PM for a more detailed discussion.
 

Jacka

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can mytalamine 40% be replaced?
 
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Methylamine cann't be substituted. If you have a lower % of methylamine, you can use it.
You can use methylamine hydrochloride instead of methylamine solution, but an alkaline solution must be added.
 
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antrax

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Methylamine cann't be substituted. If you have a lower % of methylamine, you can use it.
You can use methylamine hydrochloride instead of methylamine solution, but an alkaline solution must be added.
Marvin Popcorn SuttonMy friend, could you tell me the color and texture in it´s pure and impure state of the synthetic cathinone precursor 2-Bromo-3',4'-(methylenedioxy)propiophenone (CAS:52190-28-0)?
Most of the Chinese chemical suppliers sell it in the form of powder and small sandy brown rocks, I don't know if it has that brown color due to impurities or if it is a different chemical, since the supplier told me that said chemical precursor it has a purity of 99% even having that brown color.
thank you!!
 

ASheSChem

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possible to find in europe 3,4-methylenedioxypropiophenone or 2-bromo-3,4-methylenedioxypropiophenone ?
 

Jacka

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Methylamine cann't be substituted. If you have a lower % of methylamine, you can use it.
You can use methylamine hydrochloride instead of methylamine solution, but an alkaline solution must be added.
Marvin Popcorn SuttonAnd what alkaline solution should you combine to replace the 20ml of methylamine 40% with methylamine hydrochloride + alkaline solution that you explain in your synthesis
 

Jacka

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Can you specify the laboratory instruments that have been used in this process and the use that I play, please :)
 
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And what alkaline solution should you combine to replace the 20ml of methylamine 40% with methylamine hydrochloride + alkaline solution that you explain in your synthesis
JackaThe table shows the density of 40% methylamine as 0.89g/ cm3, hence 7.18g of pure methylamine gas is obtained in 20ml.
Let us compare the molecular weights of methylamine and its hydrochloride:
M (CH3NH2)HCl = 67.518 g/mol
M CH3NH2 = 31.057 g/mol.
Ratio = 2.174
If you use the proportions from the synthesis, you will need 15.6g of methylamine hydrochloride to replace 20ml of 40% methylamine solution.
Methylamine hydrochloride needs to be dissolved beforehand in the proportion of 1g to 2.5ml water (15.6g and 39ml).
Prepare sodium hydroxide (NaOH) solution of 18g and 54ml water, let it cool and pour it into a flask with 2-bromo-3,4-methylenedioxypropiophenone solution. After that, add methylamine hydrochloride solution. Then continue according to the instructions.
 
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Acidosis

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bk-MDMA FROM THIS METHODOLOGY AND home adaptations.
5l6eTjRPuq
 

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darkblink

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Can DCM be substituted with another solvent? How do i puchase DCM in the UK? I have Xylene and Ethyl Acetate easy available in large quantities to me
 

Mr.Blanks00

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hi, sorry friend, I want to ask, how many mg is used when used, this is used by snorting like meth or by swallowing it like a pill. Sorry, I just heard about this new thing.
 

G.Patton

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hi, sorry friend, I want to ask, how many mg is used when used, this is used by snorting like meth or by swallowing it like a pill. Sorry, I just heard about this new thing.
YusufOral way of administration
Light 75 - 150 mg
Common 150 - 225 mg
Strong 225 - 325 mg
Heavy 325 mg +
 

StarWars

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Oral way of administration
Light 75 - 150 mg
Common 150 - 225 mg
Strong 225 - 325 mg
Heavy 325 mg +
G.PattonIm can use dcm like NMP and how much need mix if on NMP need mix only 10 min then how long need mix on dcm ??
 
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G.Patton

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Is 20 minutes too short for animations?
hexenDo you understand that 10g of substance can react faster than 10 kg? There is difference and reaction time isn't constant. I have no dependence data for this (reaction load : time) reaction. As I told in previous message, you have to control it by TLC.
 

Didi

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How to made methyloamine 40% step by step ??
 

Zetetic

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Methylone (3,4-Methylenedioxymethcathinone, βk-MDMA) is a synthetic substance of the cathinone class that is often compared to MDMA. This product is very popular and causes a strong euphoria and empathy. It acts as a powerful aphrodisiac, the effect of which causes an unrestrained desire to have sex.
This article describes the synthesis of a small amount of methylone. I would like to note that the reaction scales linearly and the proportions of all substances are maintained. Methylone is quite easy to produce in large quantities. Its production does not require sophisticated laboratory equipment. This article describes the technology for producing methylone from halogen ketone (2-bromo-3,4-methylenedioxypropiophenone), which is obtained by standard bromination from 3,4-methylenedioxypropiophenone (3,4-(methylenedioxy)phenyl-1-propanone (MDP1P)).

Reagents:
  • 3,4-Methylenedioxypropiophenone (MDP1P; cas 28281-49-4) 20 g;
  • Dichloromethane (DСM) 90 ml;
  • Bromine (Br2) 22 g;
  • Sodium thiosulfate (Na2S2O3) aq solution 10% ~50 ml;
  • Distilled water;
  • n-Methylpyrrolidone (cas 872-50-4) 50 ml;
  • Methylamine aqueous 40% 20 ml;
  • Sodium bicarbonate 12 g;
  • Magnesium sulphate (MgSO4) ~30 g;
  • Hydrochloric acid (~35%) ~10 ml;
  • Acetone;
Equipment and glassware:
  • Flat bottom flask 250 ml;
  • Retort stand and clamp for securing apparatus (optional);
  • Magnetic stirrer;
  • Reflux condenser (optional);
  • Funnel;
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (500 mL x1, 250 mL x2; 100 mL x2);
  • Vacuum source;
  • Laboratory scale (0.1-200 g is suitable);
  • Measuring cylinders 100 mL;
  • Cold water bath;
  • Glass rod and spatula;
  • Separatory funnel 1 L (optional);
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Filter paper;
Synthesis procedures
MDP1P 20 g is dissolved in DСM 60 ml and a few drops of hydrochloric acid are added, then bromine 22 g is added dropwise. The reaction is exothermic, the reaction mixture is become dark, then become light by reason of hydrobromide (white gas) releasing. The remaining bromine is removed with 10% sodium thiosulfate aq solution and reaction mixture is washed with water after the end of this reaction. The organic layer can be used for the methylamination reaction (yield ~140% MDP1P) or distill off DСM under vacuum to a solid.

The synthesis is conducted under normal conditions. 2-Bromo-3,4-methylenedioxypropiophenone 10 g from previous step is dissolved with n-methylpyrrolidone 50 ml in the reaction flask. The mixture is stirred until solids are dissolved.
Methylamine aqueous 40% 20 ml is added to the mixture, the flask is closed and stirred vigorously. Exothermic reaction have to be controlled. The reaction ends in 10 min and temperature decrease.

The exothermic reaction can be very violent and a forced cooling is necessary in case of large load. The flask should be immersed into a cold water bath for cooling. It is important to keep the temperature below 55 ºC.
Methylone free base purification
The reaction mass is washed with sodium bicarbonate solution after reaction end, which is prepared in advance (water 120 ml and sodium bicarbonate 12 g). Sodium bicarbonate solution is poured into the reaction mixture and stirred vigorously for 1-2 min.
Dichloromethane (CH2Cl2) 30 ml is added and stirred vigorously for 5 min. Methylone free base is extracted by DCM from this mixture. Organic layer is separated with help of separatory funnel.
Extraction
Layers separation in separating funnel (Photo 1). The bottom layer is DCM extract with cathinone base. The aqueous fraction is top layer, which have to be separated and extracted one more time with DCM 30 ml (Photos 2-3-4). The lower organic layers are combined and washed with distilled water 60 ml 3-4 times in separatory funnel until the methylamine smell absent (Photo 5-6). Methylone free base in DCM is always in the bottom layer. Layers are separated carefully. Try to avoid getting water into the organic layer. Organic solution is dried over MgSO4.
Acidification
Methylone free base solution in DCM is diluted with an equal volume of dry acetone (Laboratory grade 99%+). Then hydrochloric acid (~35%) is added in small portions dropwise. The mixture is stirred constantly and pH is controlled. A precipitate is appeared. If the mixture became very thick, acetone is added.
The mixture must be very liquid in order to acidify methylone properly. When pH is reached 5.5-6, HCl addition is stopped. The mixture is cooled and filtered.
If methylone hydrochloride is not pure enough, you can read how to purify it here. Large crystals producing is described in this article.

Methylone hydrochloride purification with dry acetone gives a good result. There are several pictures of methylone hydrochloride before and after purification procedure.
Marvin Popcorn SuttonGreetings you and to all! Someone can suggest the result and describe the effect of the substance if 3,4-(Methylenedioxy)propiophenone is replaced in this synthesis by 3,4-(Methylenedioxy)butyrophenone.
I had such a question because I found only 3,4-(Methylenedioxy)butyrophenone in our free market.
 

G.Patton

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Greetings you and to all! Someone can suggest the result and describe the effect of the substance if 3,4-(Methylenedioxy)propiophenone is replaced in this synthesis by 3,4-(Methylenedioxy)butyrophenone.
I had such a question because I found only 3,4-(Methylenedioxy)butyrophenone in our free market.
ZeteticYou'll get 2-Methylamino-1-(3',4'-methylenedioxyphenyl)butan-1-one hydrochloride cas 17762-90-2
 
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