• The BB team is looking for employees, who are ready to work with mephedrone, amphetamine, methamphetamine and other substances.
    High wage! Stable job.

    Requirements:

    • Make a minimum deposit of 50 EUR
    • Receive a batch of goods (from 25 g and more, depending on the deposit)
    • Pack the goods in bags (1-2g) and hide them in safe places in your city.

    We going to do the rest work! As soon as the goods are sold, you'll get money for each successfully sold package!

    Relevant for all EU countries

    Contact : @Madre

William D.

Expert
Joined
Jul 19, 2021
Messages
619
Reaction score
850
Points
93
Reaction scheme:
QmU05KGcDH

Reagents:
  • 4′-Methylpropiophenone (cas 5337-93-9) 1000 g;
  • Hydrobromic acid 48% aq. 1300 g;
  • Hydrogen peroxide (H2O2) 35% 750 g;
  • Sodium bicarbonate (NaHCO3);
  • Distilled water;
Equipment and glassware:
HzO1gsfG3M

  • Three necked round bottom flask 5 L;
  • Retort stand and clamp for securing apparatus;
  • Reflux condenser;
  • Funnel;
  • Drip funnel 1 L;
  • Top stirrer;
  • Sieve filter (kitchen grade is ok);
  • Water bath;
  • Heating plate;
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (600 mL x2, 2 L, 1 L, 100 mL x2);
  • Vacuum source;
  • Laboratory scale (0.1-1000 g is suitable);
  • Measuring cylinders 1000 mL and 100 mL;
  • Glass rod and spatula;
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Filter paper;
Introduction
Bromination reaction is easily scaled under these conditions. Basic rule: hydrogen peroxide is added slowly in order to avoid the reaction mixture splashing. It is better to use a top stirrer because a magnetic stirrer doesn't cope with the sediment. Blades of stirrer must be covered with ftoroplast (Teflon) in order to avoid reactions with hydrobromic (HBr) acid.
Download Video
Synthesis:
1. 4'-Methylpropiophenone 1000 g is added into a flask.
2. Hydrobromic (HBr) acid 1300 g 48% is poured into the flask and stirred for 5 min.
3. Hydrogen peroxide 750 g 35% is added into a drip funnel 1 l.
4. Hydrogen peroxide is added dropwise to the stirred reaction mixture.
5. Bromine is released during hydrogen peroxide addition to the mixture, dissolved in solution and reacted.
6. Hydrogen peroxide must be added at an appropriate rate so that the reaction mixture becomes colorless.
7. Reaction mixture temperature have to be kept less than 65 °C. An external cooling is applied in case of overheating. If reaction temperature is higher, hydrogen peroxide addition is stopped.
8. The second part of discoloration reaction can be conducted for longer time. Hydrogen peroxide is added according with reaction temperature.
9. Reaction mixture is left for a 12 h with a constant stirring at room temperature as soon as all hydrogen peroxide is added.
10. After 12 h precipitate is formed.
11. Sodium bicarbonate aq solution is added to the reaction mixture to reach neutral pH 6-7, stir it well. The mixture with 2-bromo-4'-methylpropiophenone is filtered through a Buchner funnel. Product is washed with small amount of distilled water.
12. Crude 2-bromo-4'-methylpropiophenone (cas 1451-82-7) is used for further reactions. Theoretical yield up to 1530 g. Practice yield is almost quantitative (video yield 94%).
 
Last edited by a moderator:

dk77

Don't buy from me
Member
Joined
Feb 27, 2022
Messages
7
Reaction score
0
Points
1
Reaction sheme:
View attachment 1290

Reagents:
4-methylpropiophenione 1000 g,
Hydrobromic acid 48% aq. soln. 1300 g,
Hydrogen peroxide 35% 750 g,
Baking soda,
Water.

Preamble:
The bromination reaction is easily scaled under these conditions. Basic rule - add peroxide slowly to avoid splashing the reaction mixture. In the role of a mixing device, it is better to use the overhead stirrer, the magnetic stirrer does not cope with the sediment. The blades of the mixers must be covered with teflon to avoid reactions with HBr acid.

Synthesis:
1. 1000 g 4-methylpropiophenone added to the flask.
2. 1300 g 48% HBr acid poured in flask and stir 5 minutes.
3. 750 g 35% hydrogen peroxide added to the drip funnel.
4. Dropwise hydrogen peroxide to the stirred reaction mixture.
5. In the process of adding peroxide in the mixture, a bromine is released, and with stirring dissolves reacting.
6. It is necessary to add at a rate such that the bromine discolored.
7. Control the temperature of the reaction (>75 *C), we do not give boiled mixtures.
8. The second half of the reaction discoloration can go longer, add peroxide, focusing on temperature growth.
9. How all the peroxides added, leave the reaction to night on stirring at room temperature.
10. The next day, we see precipitation.
11. Add a saturated soda aqueous solution, drain the water from the sediment from the flask through the sieve, rinse with re-clean water.
12. Use the crude bromoketone for further reactions with theoretical calculation of the yield until 1500 g.
William DampierAnother hydrobromic acid synthesized by Hans-Dietrich is 780ML, here 1300 hydrobromic acid. What is the difference between oxidizing liquid 136ML and 750ML?
 

William D.

Expert
Joined
Jul 19, 2021
Messages
619
Reaction score
850
Points
93
1300 g (or 1L) aq. HBr 48% - 1,2eq for 4-methylpropiophenone
 
Last edited by a moderator:

dk77

Don't buy from me
Member
Joined
Feb 27, 2022
Messages
7
Reaction score
0
Points
1
Sorry, when the hydrogen oxide reaches 500 grams it turns red instead of changing color, then a deeper red when added. Need to finish adding?
 
Last edited:

William D.

Expert
Joined
Jul 19, 2021
Messages
619
Reaction score
850
Points
93
Sorry, when the hydrogen oxide reaches 500 grams it turns red instead of changing color, then a deeper red when added. Need to finish adding?
dk77Continue stirring until discoloration. If no discoloration occurs, stop the reaction. The proportions given are those with an excess of hydrobromic acid and peroxide, but they may be reduced (1,1KG HBr48% and 0,65KG H2O2)
 

dk77

Don't buy from me
Member
Joined
Feb 27, 2022
Messages
7
Reaction score
0
Points
1
Continue stirring until discoloration. If no discoloration occurs, stop the reaction. The proportions given are those with an excess of hydrobromic acid and peroxide, but they may be reduced (1,1KG HBr48% and 0,65KG H2O2)
William DampierSince English is not my native language, I may not express well. I mean, when it starts dripping, it changes color and then becomes transparent, but after the critical point it becomes opaque and the whole thing turns red. Is it time to stop? Is it bad to add too much hydrogen peroxide? I stop when he turns red and can't change color because I don't know when to stop, then once the temperature drops, crystals form. I don't know if this is 2-bromo-4-methylpropiophenone. I will add pictures later. thank you for your help.
 
Last edited:

William D.

Expert
Joined
Jul 19, 2021
Messages
619
Reaction score
850
Points
93
Since English is not my native language, I may not express well. I mean, when it starts dripping, it changes color and then becomes transparent, but after the critical point it becomes opaque and the whole thing turns red. Is it time to stop?
dk77Not always, maybe you need more time, oriented on the proportion above
Is it bad to add too much hydrogen peroxide?
No problems, anything, excess will not hurt
I stop when he turns red and can't change color because I don't know when to stop, then once the temperature drops, crystals form. I don't know if this is 2-bromo-4-methylpropiophenone.
These crystals - 2-bromo-4-methylpropiophenone
 

hlebsladky2

Don't buy from me
New Member
Joined
Apr 10, 2022
Messages
12
Reaction score
3
Points
3
Reaction sheme:
View attachment 1290

Reagents:
4-methylpropiophenione 1000 g,
Hydrobromic acid 48% aq. soln. 1300 g,
Hydrogen peroxide 35% 750 g,
Baking soda,
Water.

Preamble:
The bromination reaction is easily scaled under these conditions. Basic rule - add peroxide slowly to avoid splashing the reaction mixture. In the role of a mixing device, it is better to use the overhead stirrer, the magnetic stirrer does not cope with the sediment. The blades of the mixers must be covered with teflon to avoid reactions with HBr acid.

Synthesis:
1. 1000 g 4-methylpropiophenone added to the flask.
2. 1300 g 48% HBr acid poured in flask and stir 5 minutes.
3. 750 g 35% hydrogen peroxide added to the drip funnel.
4. Dropwise hydrogen peroxide to the stirred reaction mixture.
5. In the process of adding peroxide in the mixture, a bromine is released, and with stirring dissolves reacting.
6. It is necessary to add at a rate such that the bromine discolored.
7. Control the temperature of the reaction (>75 *C), we do not give boiled mixtures.
8. The second half of the reaction discoloration can go longer, add peroxide, focusing on temperature growth.
9. How all the peroxides added, leave the reaction to night on stirring at room temperature.
10. The next day, we see precipitation.
11. Add a saturated soda aqueous solution, drain the water from the sediment from the flask through the sieve, rinse with re-clean water.
12. Use the crude bromoketone for further reactions with theoretical calculation of the yield until 1500 g.
William DampierWhat does a crude bk4 look like? Btw, to do methylamination should I wait to the whole substance to become crystal or I can skip waiting for a night?
 

William D.

Expert
Joined
Jul 19, 2021
Messages
619
Reaction score
850
Points
93
What does a crude bk4 look like? Btw, to do methylamination should I wait to the whole substance to become crystal or I can skip waiting for a night?
hlebsladky2Wait for the crystallization of the substance. Raw and washed looks the same as dry, only wet
 

hlebsladky2

Don't buy from me
New Member
Joined
Apr 10, 2022
Messages
12
Reaction score
3
Points
3
Reaction sheme:
View attachment 1290

Reagents:
4-methylpropiophenione 1000 g,
Hydrobromic acid 48% aq. soln. 1300 g,
Hydrogen peroxide 35% 750 g,
Baking soda,
Water.

Preamble:
The bromination reaction is easily scaled under these conditions. Basic rule - add peroxide slowly to avoid splashing the reaction mixture. In the role of a mixing device, it is better to use the overhead stirrer, the magnetic stirrer does not cope with the sediment. The blades of the mixers must be covered with teflon to avoid reactions with HBr acid.

Synthesis:
1. 1000 g 4-methylpropiophenone added to the flask.
2. 1300 g 48% HBr acid poured in flask and stir 5 minutes.
3. 750 g 35% hydrogen peroxide added to the drip funnel.
4. Dropwise hydrogen peroxide to the stirred reaction mixture.
5. In the process of adding peroxide in the mixture, a bromine is released, and with stirring dissolves reacting.
6. It is necessary to add at a rate such that the bromine discolored.
7. Control the temperature of the reaction (>75 *C), we do not give boiled mixtures.
8. The second half of the reaction discoloration can go longer, add peroxide, focusing on temperature growth.
9. How all the peroxides added, leave the reaction to night on stirring at room temperature.
10. The next day, we see precipitation.
11. Add a saturated soda aqueous solution, drain the water from the sediment from the flask through the sieve, rinse with re-clean water.
12. Use the crude bromoketone for further reactions with theoretical calculation of the yield until 1500 g.
William DampierHey! How much should I add of a saturated soda aqueous solution? Thanks.
 

William D.

Expert
Joined
Jul 19, 2021
Messages
619
Reaction score
850
Points
93
Hey! How much should I add of a saturated soda aqueous solution? Thanks.
hlebsladky2We look when the reaction has ceased to discolor. After this and crystallization of the product, we can add dry soda. Add while stirring in small portions until the red color disappears and the reaction stops bubbling.
 

hlebsladky2

Don't buy from me
New Member
Joined
Apr 10, 2022
Messages
12
Reaction score
3
Points
3
We look when the reaction has ceased to discolor. After this and crystallization of the product, we can add dry soda. Add while stirring in small portions until the red color disappears and the reaction stops bubbling.
William DampierThanks! As for the distilled water to add, should it be equal to the reagent volume?
 

William D.

Expert
Joined
Jul 19, 2021
Messages
619
Reaction score
850
Points
93
Thanks! As for the distilled water to add, should it be equal to the reagent volume?
hlebsladky2It does not matter, you can add water to the entire volume of the flask, but at least one equivalent of the volume of the reaction mixture
 

ZhengJi

Don't buy from me
Member
Joined
May 15, 2022
Messages
4
Reaction score
0
Points
1
Which solvent is best for recrystallization 2-bromo-4'-methylpropiophenone? I have tried this method but my 2b4mpp is a little bit dirty - white instead of colorless cristal.
 

dk77

Don't buy from me
Member
Joined
Feb 27, 2022
Messages
7
Reaction score
0
Points
1
Which solvent is best for recrystallization 2-bromo-4'-methylpropiophenone? I have tried this method but my 2b4mpp is a little bit dirty - white instead of colorless cristal.
ZhengJiPost a photo and I'll see if it's the right product
 

dk77

Don't buy from me
Member
Joined
Feb 27, 2022
Messages
7
Reaction score
0
Points
1
Which solvent is best for recrystallization 2-bromo-4'-methylpropiophenone? I have tried this method but my 2b4mpp is a little bit dirty - white instead of colorless cristal.
ZhengJiHave you ever bought or produced a transparent and colorless product?
 

William D.

Expert
Joined
Jul 19, 2021
Messages
619
Reaction score
850
Points
93
Which solvent is best for recrystallization 2-bromo-4'-methylpropiophenone? I have tried this method but my 2b4mpp is a little bit dirty - white instead of colorless cristal.
ZhengJiWhite color is good for this, it should not be transparent (although large crystals grow under some conditions)
 

ADATA

Don't buy from me
Resident
Joined
Jun 6, 2022
Messages
21
Reaction score
5
Points
3
7. Reaction mixture temperature have to be maintained higher 75 °C but less than boiling temperature

It seems to have to be lower than 75C before
So it is correct to be higher than 75C?
 

ADATA

Don't buy from me
Resident
Joined
Jun 6, 2022
Messages
21
Reaction score
5
Points
3
Can anyone answer me whether it is correct to say that it is above 75 degrees C and below the boiling point?
The previous data was 65 degrees C
 

ADATA

Don't buy from me
Resident
Joined
Jun 6, 2022
Messages
21
Reaction score
5
Points
3
Synthesis of mephedrone (4-MMC) from haloketones in ethyl acetate. 1-10 kg scale.

The temperature mentioned here is not to exceed 65 degrees
I'm confused
 
  • Free product samples

    Testing products from new vendors and manufacturers.

    Get free samples for testing now!

  • Always stay in touch with BB forum. Element/Matrix.

    Connect notifications to always stay in touch with the forum!

    Connect

  • The BB Forum team is looking for cooperation:

    • Traffic arbitrage specialists
    • Spammers
    • Advertising agencies
    • Bloggers/Vloggers
    • TOR sites directories
    • Creative people who can create viral content
    • Administrators of Telegram Channels and Groups

      We will pay more for your traffic than our competitors! $0.1 per visitor!!!If you are interested in, write to the administrator.
Top