4-MMC (mephedrone) synthesis in DCM

SonicNL

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I've tried this synthesis and gotten yields ranging from 30% 45%. Sharing in case it might be helful to others. Vice versa, other people might know changes to this synthesis for higher yields.

Improvements are always welcome

Needed:
100 g 2-bromo-4-methylpropiophenone
500 ml DCM
200 ml Methylamine 40% aqua solution
60 ml HCI 30÷ aqua solution
550 ml Acetone
2 L Deminiralised water
PH measuring Strips
1 L IPA

Equipment:
Round bottom flask 2 L
Hotplate
Measuring cups 1 L
Crystallization dish
Vacuum pump
Buchner flask

1. Add 100 g 2-bromo-4-methylpropiophenone to 500 ml DCM and let it dissolve.
2. Add 200 ml methylamine in 4 portions
3. After 30 mins, put on hotplate and stir.
4. Temperature 32-36 C for 4 hours, or 40 C for 2 hours.
5. Rinse in measuring cup with demi-water until there is no methylamine smell left. Stir or shake after adding.
6. Add an ice cold solution of acetone/HCI 550ml/60ml, or add ice cold acetone and add HCI after.
7. Measure the PH, should be 6.
7. Put the 4-MMC freebase in freezer for 12h
8. Rinse with ice cold acetone trough buchner filter.
9. If you have obtained dry 4-MMC prepare a solution of 50/50 demi-water and IPA. Add 1g per 2-3 ml solvent. Boil until 4-MMC (Not longer than needed, aprox. 1-3 min.). Pour into a crystallization dish. When crystallization stops at room temperature, put the dish in the fridge. Put in freezer after and you will be left with nice looking crystals.
 

SonicNL

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@HerrHaber this is the method i've been using so far.
 

SonicNL

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Wet crystal
 

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pachemguy

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That's some fine crystal you got there ican smell it threw the screen already 😄 4mmc was to me at least never rreally popular here in the USA but a I purchased a few kgs before it got put on ban sadly gone but dearly missed. But 4mmc absolutely next on my list as soon. As I finish up the a-pvp Synth. So you purchase the bromoketone skipping the bromonatio. All together? I found a few seemingly good sources for methylpropiophenone but I could never find the 2 bromo species that would be awesome!
 

SonicNL

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Thanks. It sure does have a smell. I was not satisfied though, so I repeated the washing and crystallization procedure.

Yes, I'm trying to avoid working with bromine. And yeah my suplier provides high quality bromoketone and they know how to ship.
 

w2x3f5

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4 point. at 35 degrees the reaction takes place in two hours, at 40 degrees there will be more impurities. What is the yield of powder? The crystal is dirty.
 

SonicNL

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You are wrong. Its 4 h on 35 c
Read instead of only looking at my crystal. Ur anwsers are in my posts lol.
 
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w2x3f5

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Sorry, I didn't notice the release of the substance. Now I see it frustrating 35-45.
 

OttoBulletproof

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In other synthesis NMP is also used. Is it not actually necessary? Will not using it reduce yields?
 

Sailor

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SonicNL

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Hey, late reply but to answer your question:
No, adding benzene is not neccessary as DCM is the solvent instead of benzene. Benzene is more carcinogenic than DCM.

I havent tried NMP and im no expert maybe someone else can answer this.
 

Dexterror

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Why hcl 30% not 35-38 % ?
 

UWe9o12jkied91d

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Because it works just the same and is cheaper/easier to find probably
 
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Heineken

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yes is much country is hard to found 35-38% acid
 

UWe9o12jkied91d

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Ye, you can also find silyl chlorides to make anhydrous hcl or buy in ether or methanol.
 

TheVacuumGuy

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Searched for this but couldn't find usable info. Could you elaborate?
 

Dexterror

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no reflux condenser needed for this synthesis? Dcm heated to 40 degrees (boiling point) can sometimes lead to an explosion heated for such a time at such a temperature in a closed flask?
 
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UWe9o12jkied91d

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it's better praxis to use a condenser with a balloon or glove covering the exit, it's not necessary to stopper tight
I do this synthesis in DCM and use 0 heat, just good stirring and left overnight
 

Dexterror

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But if I do this synthesis with heating to 40 degrees with a closed flask, an explosion is possible?
 

UWe9o12jkied91d

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probable rather than possible I would say, if the whole mass is at 40C in a closed glass system
the author's probably he's just SET it to 40C without measuring the temp of the mass or maybe I'm underestimating him
 

TheVacuumGuy

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It could be me, but read nowhere a closed flask was used. And why would you? Closed flask if pressure becomes too high the stopper will pop off nothing more nothing less
 

TheEnthusiasticCat

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Build up of pressure if you seal completely, I would recommend having slightly ajar to prevent build up of pressure and also to contain any fumes / smells, of course extraction of some sort is recommended. I'm comfortable using a temperature between 38°C to 40°C when performing a 4MMC synthesis using DCM. Or you can do 0°C for 18 to 24 hours, 24 hours would be preferable.
 
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