• 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 and UK

    Contact : @Madre

G.Patton

Expert
Joined
Jul 5, 2021
Messages
2,387
Solutions
3
Reaction score
2,327
Points
113
Deals
1
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
ADATAHello, sorry for a late reply. Temperature have to be less than 65 *C. I fixed this mistake, I apologize.
 
Last edited:

Zetetic

Don't buy from me
New Member
Joined
Dec 2, 2022
Messages
18
Reaction score
4
Points
3
Hello, sorry for a late reply. Temperature have to be less than 65 *C. I fixed this mistake, I apologize.
G.PattonGreetings, dear G. Patton! Please pay attention to my question in this thread. You, in my opinion, are one of the most attentive and prompt experts among all forum participants.
p. s. I ask other forum members not to take offense at my words ;-)
 

Zetetic

Don't buy from me
New Member
Joined
Dec 2, 2022
Messages
18
Reaction score
4
Points
3
Reaction scheme:

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: View attachment 7238
  • 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%).
William DampierHello dear! If I use propiophenone and not 4-methylpropiophenone, do I need to change anything in this method? I hope to get bc-1 this way. And in the next step, from bq-1, through the method with ethyl acetate, acetone and hydrochloric acid, obtain an ephedron salt. Am I on the right track?
 

G.Patton

Expert
Joined
Jul 5, 2021
Messages
2,387
Solutions
3
Reaction score
2,327
Points
113
Deals
1
Hello dear! If I use propiophenone and not 4-methylpropiophenone, do I need to change anything in this method? I hope to get bc-1 this way. And in the next step, from bq-1, through the method with ethyl acetate, acetone and hydrochloric acid, obtain an ephedron salt. Am I on the right track?
ZeteticYou have to recount reagent amounts according molecular weight of propiophenone.
Moles, grams, litres and chemical calculations
 

DavidNichols

Don't buy from me
New Member
Joined
Mar 7, 2023
Messages
14
Reaction score
14
Points
3
Reaction temperature of 65 °C is simply wrong, since 2-bromo-4'-methylpropiophenone forms of crystals and lock 4′-methylpropiophenone inside. 2b-4m melting temperature is about 77 °C and it is very far from HBr boiling point. Consequently, 75-85 °C is a sweet range for your reaction temperature that should complete your halogenation roughly in 2 hours. The questions to answer:

1. will position of a bromine be right or you end with iso-mephedrone after amination?
2. will fraction of stereoisomers will be still 50:50 in this method?
 

w2x3f5

Don't buy from me
Resident
Joined
Jan 15, 2023
Messages
339
Reaction score
150
Points
43
Reaction temperature of 65 °C is simply wrong, since 2-bromo-4'-methylpropiophenone forms of crystals and lock 4′-methylpropiophenone inside. 2b-4m melting temperature is about 77 °C and it is very far from HBr boiling point. Consequently, 75-85 °C is a sweet range for your reaction temperature that should complete your halogenation roughly in 2 hours. The questions to answer:

1. will position of a bromine be right or you end with iso-mephedrone after amination?
2. will fraction of stereoisomers will be still 50:50 in this method?
DavidNicholsat elevated temperatures, side reactions are more likely, it is much better to carry out bromination in a solvent.
The question also arises about the decomposition of hydrogen peroxide at elevated temperatures, it is better to choose a replacement for this oxidizing agent.
so bromination without solvent and below the halogen ketone crystallization temperature is a very bad idea, there are complaints on the forum about the supplier of dirty halogen ketone in which there is a large admixture of the original ketone.
 

DavidNichols

Don't buy from me
New Member
Joined
Mar 7, 2023
Messages
14
Reaction score
14
Points
3
at elevated temperatures, side reactions are more likely, it is much better to carry out bromination in a solvent.
The question also arises about the decomposition of hydrogen peroxide at elevated temperatures, it is better to choose a replacement for this oxidizing agent.
so bromination without solvent and below the halogen ketone crystallization temperature is a very bad idea, there are complaints on the forum about the supplier of dirty halogen ketone in which there is a large admixture of the original ketone.
w2x3f5I agree with you on using solvent for more even halogen distribution. H2O2 decomposition is unlike happen unless you reflux it up to 120-130 °C. The main issue is you having all the condition for di- and tri-halogenation. Stereo parity is also questioned, but its a pure speculation.
 

w2x3f5

Don't buy from me
Resident
Joined
Jan 15, 2023
Messages
339
Reaction score
150
Points
43
I agree with you on using solvent for more even halogen distribution. H2O2 decomposition is unlike happen unless you reflux it up to 120-130 °C. The main issue is you having all the condition for di- and tri-halogenation. Stereo parity is also questioned, but its a pure speculation.
DavidNicholsLet's start with the fact that hydrogen peroxide self-decomposes over time during storage, naturally, the higher the temperature, the faster the decomposition, as well as local overheating when adding peroxide, where the temperature is much higher than the temperature of the reaction mass itself. Do not trust me, you can attach an empty bag to a reflux condenser and see how much oxygen is released from the decomposition of peroxide.
All conditions for polyhalogenation creates an excess of acid and the need to use peroxide in excess. I gave up peroxide a long time ago, it is the worst oxidizing agent for this reaction.
 

ADATA

Don't buy from me
Resident
Joined
Jun 6, 2022
Messages
21
Reaction score
6
Points
3
The 2B4M produced in this way has a lot of impurities. I'm not sure what it is, the follow doesn't work
 

Lev

Don't buy from me
Resident
Joined
Mar 14, 2023
Messages
8
Reaction score
9
Points
3
Good afternoon, tell me if it is possible to replace 4-methyloprofenone with another reagent
2-(1-bromoethyl)-2-(4-methylphenyl)-1,3-dioxolan ?
 

w2x3f5

Don't buy from me
Resident
Joined
Jan 15, 2023
Messages
339
Reaction score
150
Points
43
Good afternoon, tell me if it is possible to replace 4-methyloprofenone with another reagent
2-(1-bromoethyl)-2-(4-methylphenyl)-1,3-dioxolan ?
Levhydrolysis of dioxalane up to 2b4m and further amination
maybe can do first amination after do hydrolysis, its need check in small amount
 
Last edited:

Lev

Don't buy from me
Resident
Joined
Mar 14, 2023
Messages
8
Reaction score
9
Points
3
Bromdioxolane 98%
 

w2x3f5

Don't buy from me
Resident
Joined
Jan 15, 2023
Messages
339
Reaction score
150
Points
43
Bromdioxolane 98%
Levnew replacement 2b4m, obtained by conducting a halogenation reaction in a solution of ethylene glycol, standard protecting group for ketone
 
  • 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