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WillD

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Selassi

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Okay thank you
 

Selassi

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We already did a succesfull synthesis of 3cmc. The help was greatly appreciated.
 

Epikureetsdrug

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We already did a succesfull synthesis of 3cmc. The help was greatly appreciated.
SelassiMy congratulations, friend! You're the best! After such great success in subjugating substances, could you share with your fans your unique experience of this synthesis? because I've been trying for about a month to get a meager but successful result in 3cmc synthesis, but so far I've only had fiascos. I have already tried 5 different solvents, I personally dried acetone by distillation and with anhydrous magnesium sulfate, but after acidification and daily exposure of the glass 🥛with the product at🌡️ -20⁰C, there was not even a hint of crystallization. Tell me the CAS number of the starting substance at the beginning, please?
 

Selassi

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Here is the result of the 3cmc
 

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Yavuz1453

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sir, i want to make it at home alone. can it be made in a pot and what material should i buy please help me if you can help me saddle i would be very grateful thank you
 

Lucy123

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Reaction scheme:
View attachment 1218

Reagents:

2-bromo-4-methylpropiophenone (BK4) - 5 kg;
n-methyl-2-pyrrolidone (NMP) - 20 L;
Methyl amine 40% aq.soln - 8 L;
Benzene - 15 L;
Acetone - 30 L;
Hydrochloric acid con.aq.soln ~ 1,5 L.

Synthesis:
1. 5 kg 2-bromo-4-methylpropiophenone (BK4) added to the reactor or have calculated amount of crude BK4 after halogenation reactions.
2. 20 liters n-methyl-2-pyrrolidone poured, start stirring and heating to 40 *C.
3. Upon reaching 40 *C within the mixture, pour 8 liters methyl amine 40% aq.soln and continue stirring 20 minutes.
4. Next, we pour 20 liters of clean cold water, stirring a few minutes.
5. Pour 15-20 liters benzene or other suitable extractor, stirring a few minutes.
6. Stop stirring, waiting for the separation of the mixture into two layers.
7. The bottom aqueous layer was drained through the bottom valve of the reactor.
8. 20 liters of ice acetone was poured and add hydrochloric acid with stirring to pH - 5
9. Overload the mixture in the freezer.
10. Filter on the nutshe-filter, dry.

Notes:
NMP can be replaced by DMSO, DMF, Sulfolane.
William DampierHello William,
Changing 2-bromo-4-methylpropiophenone with 2
bromo, 3-chloropropiophenone will get me 3cmc. Many thanks!
 

Lucy123

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SelassiThanks Selassy! I guess I should keep the same proportions for the other substances? I must admit I don't have any chemistry knowledge.
And a other question: How should I cristalaze the final result? I really appreciate all your help!
 

Selassi

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Yes u can use the same amounts and proportions.
 

Khaafii

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Reaction scheme:
View attachment 1218

Reagents:

2-bromo-4-methylpropiophenone (BK4) - 5 kg;
n-methyl-2-pyrrolidone (NMP) - 20 L;
Methyl amine 40% aq.soln - 8 L;
Benzene - 15 L;
Acetone - 30 L;
Hydrochloric acid con.aq.soln ~ 1,5 L.

Synthesis:
1. 5 kg 2-bromo-4-methylpropiophenone (BK4) added to the reactor or have calculated amount of crude BK4 after halogenation reactions.
2. 20 liters n-methyl-2-pyrrolidone poured, start stirring and heating to 40 *C.
3. Upon reaching 40 *C within the mixture, pour 8 liters methyl amine 40% aq.soln and continue stirring 20 minutes.
4. Next, we pour 20 liters of clean cold water, stirring a few minutes.
5. Pour 15-20 liters benzene or other suitable extractor, stirring a few minutes.
6. Stop stirring, waiting for the separation of the mixture into two layers.
7. The bottom aqueous layer was drained through the bottom valve of the reactor.
8. 20 liters of ice acetone was poured and add hydrochloric acid with stirring to pH - 5
9. Overload the mixture in the freezer.
10. Filter on the nutshe-filter, dry.

Notes:
NMP can be replaced by DMSO, DMF, Sulfolane.
William DampierWhat step should I undergo if I still have to react the bromine with the 4-methylpropiophenone. In what quantity for this scale? I also need benzene for that, right?
 

rickyrick

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Is there a substitute that can be used instead of benzene?its highly carcenogenic and volatile.if not is there a viable synth of it large scale.sodium benzonate and sodium hydroxide destillation doesnt seem viable to me for large scale.importing it only option?thanks.
 

Khaafii

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What is the theoretical yield mephedrone of this synthesis scheme?
 

rickyrick

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Can benzene be substituted with toluene?
 

KWasd

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Hello, I have been testing this synthesis and have a few questions about it:

1. when adding methylamine 40% in point 3, do you add it all at once, or in small portions making sure the mixture does not exceed 60 degrees?

2. point 4 mentions cold pure water, can it be cooled with dry ice to these 3-5 degrees C?

3. point 8 mentions ice-cold acetone, can I add a large amount of dry ice to it to cool it to -30 / -50 degrees C?

4. point 9 mentions putting the whole thing in the freezer, what is the purpose of this and is it necessary?


In general, I tested this synthesis, I must admit that it works and is fabulously simple, no less I used acetone at 5-10 degrees C, making the final product blue and impossible to rinse. I think it has to do with the warm acetone, at point 8, making a dimmer or some other form of impurity. Do I understand this correctly?

I would like to ask someone in the subject to answer as to the above 4 questions. Greetings
 

G.Patton

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Hi.
small portions making sure the mixture does not exceed 60 degrees?
KWasdof course this
point 4 mentions cold pure water, can it be cooled with dry ice to these 3-5 degrees C?
yes, but your water will turn to ice
point 8 mentions ice-cold acetone, can I add a large amount of dry ice to it to cool it to -30 / -50 degrees C?
Yes, but you don't need to use so cold acetone. -5-10 *C Is enough
point 9 mentions putting the whole thing in the freezer, what is the purpose of this and is it necessary?
The purpose is crystallization. Low temperature helps to form crystals of mephedrone from solution.
 
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