4-MMC (mephedrone) synthesis in DCM

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If you are looking for a reliable supplier of hard-to-find chemicals, Brumer is the right choice. Brumer is a reliable supplier.

Nitroethane, methylamine, benzaldehyde, methylpropiophenone, 2-bromo-4-methylpropiophenone, 2-iodo-4-methylpropiophenone are already available. Shipping worldwide! flexible payment terms, safe delivery. We take into account the wishes of customers and even offer discounts!

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If you are looking for a reliable supplier of hard-to-find chemicals, Brumer is the right choice. Brumer is a reliable supplier.

Nitroethane, methylamine, benzaldehyde, methylpropiophenone, 2-bromo-4-methylpropiophenone, 2-iodo-4-methylpropiophenone are already available. Shipping worldwide! flexible payment terms, safe delivery. We take into account the wishes of customers and even offer discounts!

I will give you the best offer. Write me
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Dexterror

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Why hcl 30% not 35-38 % ?
 

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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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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?
Dexterrorit'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
 

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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
UWe9o12jkied91dBut if I do this synthesis with heating to 40 degrees with a closed flask, an explosion is possible?
 

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

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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?
DexterrorIt 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
 

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If 40 percent methylamine solution is not available, can 15 percent be used? Would one just use 2.5 times more? For example if 200ml of 40% is needed, use 500ml of 15%.

Would the other reagents or solvents need an increase also? Or could those stay the same?
 

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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.
SonicNLthe yield of said 4-MMC chemical synthesis route, with 30-45% do you mean the yield of mephedrone crystals after recrystalization?
Thank you!!
 

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the yield of said 4-MMC chemical synthesis route, with 30-45% do you mean the yield of mephedrone crystals after recrystalization?
Thank you!!
antraxIt's possible he is not calculating yields by moles, with 24h reaction time in DCM at rt. yields are very good, above 40% for sure after crystalization
 

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4mmc hcl
 

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SonicNL

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Images
Bk4 in dcm
WZg1S3hbQT


Freebase after 3h, needs washing
6rMwgd35BC


Pure freebase before acidification
WoqRvD6Uae


4-MMC after adding acid pH 5
94ZHk3Dbmw
 

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experimentsci

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Hallo guys,
I also prefer method in DCM.
I mixed 100g of Bromketon in 300ml DCM and slowly added 200ml of Methylamin 40%a.q. solution.

Now my question, what temperature and what time would be the best.
Last time I kept temperature at 36 - 37 degrees and reaction-time was 3hours.
But the product was extremly blue after acification.

How can I repair the relation between temperature and cooking time best.
Smaller temperature = longer reaction time?

Which temperature are not working.

Can anybody help and explain the reasons of temperature and cooking time?

Thank you a lot.
 

TheVacuumGuy

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Hallo guys,
I also prefer method in DCM.
I mixed 100g of Bromketon in 300ml DCM and slowly added 200ml of Methylamin 40%a.q. solution.

Now my question, what temperature and what time would be the best.
Last time I kept temperature at 36 - 37 degrees and reaction-time was 3hours.
But the product was extremly blue after acification.

How can I repair the relation between temperature and cooking time best.
Smaller temperature = longer reaction time?

Which temperature are not working.

Can anybody help and explain the reasons of temperature and cooking time?

Thank you a lot.
experimentsciMy experience is that you can easily do it at 40 (rm temp! Use glass thermometer which goes into your mixture). DCM seems very reluctant to start actually boiling (like it has some buffer zone of sorts). If I increase temp it stubbornly keeps sitting at 40.

Either way. That relation time/temp thing is only important for those in a constant hurry. The fact that a reaction takes a certain time doesn't mean you need to stopwatch tightly. Product doesn't walk away. On 35 overnight, 25 overnight, 40 in 2 hours, 40 in 8 hours . you'll get the same output (where, imho, longer = better).
 
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TheVacuumGuy

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u use 400g 2b4m and u get 400g powder 4mmc ??
$!$265,5.
The reaction I did shortly thereafter was one from 200g but used 800 dcm. This one yielded 165g. So that's around 75 percent (when accounted for some losses during crystallize). Much better than the one where used too little DCM.

So the 6 hour reaction I have to admit it didnt work as good (for future readers)
 

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265,5.
The reaction I did shortly thereafter was one from 200g but used 800 dcm. This one yielded 165g. So that's around 75 percent (when accounted for some losses during crystallize). Much better than the one where used too little DCM.

So the 6 hour reaction I have to admit it didnt work as good (for future readers)
TheVacuumGuy2h 40° to najlepszy sposób na dcm true.
A lot u lost when u wash it acetone much product is still on dcm when u wash it
 

w2x3f5

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Hallo guys,
I also prefer method in DCM.
I mixed 100g of Bromketon in 300ml DCM and slowly added 200ml of Methylamin 40%a.q. solution.

Now my question, what temperature and what time would be the best.
Last time I kept temperature at 36 - 37 degrees and reaction-time was 3hours.
But the product was extremly blue after acification.

How can I repair the relation between temperature and cooking time best.
Smaller temperature = longer reaction time?

Which temperature are not working.

Can anybody help and explain the reasons of temperature and cooking time?

Thank you a lot.
experimentsciYou have a problem with bromoketone, most likely it is dirty. you need to watch its melting point and try to recrystallize the bromoketone, or you will have aniline homologues mixed with mmc
 
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You have a problem with bromoketone, most likely it is dirty. you need to watch its melting point and try to recrystallize the bromoketone, or you will have aniline homologues mixed with mmc
w2x3f5How to do.it ??
 
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