4-MMC (mephedrone) synthesis in DCM

[Dexterror]

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?

 

[TheEnthusiasticCat]

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.

 

[experimentsci]

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]

My 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).

 

[$!$]

form 1kg 2b4m 400g 4mmc powder or crystal ?? wow
i was get much year a go 880g powder 820g crystal on dcm now for me 600g crystal is better who i do all my work in 2h crystal i made on now the same day.All info how to made u have on forum if u know somting about chemistry

 

[TheVacuumGuy]

Read again

 

[$!$]

u use 400g 2b4m and u get 400g powder 4mmc ??

 

[TheVacuumGuy]

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)

 

[$!$]

2h 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

 

[4synergy]

Meph in DCM

 

[TheEnthusiasticCat]

I think 300ml DCM is plenty for this amount of BK4, 500ml in my opinion is too much and you could be saving money instead.

How long does your crystallisation take out of curiosity?

Hope you're well.

 

[4synergy]

Took 1 day for me

 

[TheEnthusiasticCat]

Can I see your crystals please?

 

[4synergy]

https://imgur.com/8eJDFAB

 

[TheEnthusiasticCat]

[4synergy]

Thank you, i can see your crystals?

 

[Albert13]

How do you get crystals so quickly?

 

[4synergy]

with the cold method and 50/50 IPA and d-water

 

[Albert13]

Do you mean crystallization in the refrigerator?

 

[4synergy]

Yes