4-MMC (mephedrone) synthesis in DCM

experimentsci

Don't buy from me
Resident
Joined
Dec 17, 2023
Messages
17
Reaction score
3
Points
3
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

Don't buy from me
Resident
Joined
Sep 20, 2023
Messages
58
Reaction score
16
Points
8
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).
 
View previous replies…

experimentsci

Don't buy from me
Resident
Joined
Dec 17, 2023
Messages
17
Reaction score
3
Points
3
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).
TheVacuumGuyThank you very much for your answer. I am just afraid, that, when I let everything react longer, that more side-products will increse and impury my product.
My last batch, I washed out the blue colour with acetone during filtering. I will send product to a labor to check, if it is good.

I also checked, that I used a little to much Methylamine. For 100g Bromketone I added 200ml Methylamine 40%a.q. solution.
I think 160ml should be enough (after calculation 1mol Bromketone vs. 2 moles Methylamine and a little buffer for Methylamine)
 
  • Like
Reactions: $!$

TheVacuumGuy

Don't buy from me
Resident
Joined
Sep 20, 2023
Messages
58
Reaction score
16
Points
8
Thank you very much for your answer. I am just afraid, that, when I let everything react longer, that more side-products will increse and impury my product.
My last batch, I washed out the blue colour with acetone during filtering. I will send product to a labor to check, if it is good.

I also checked, that I used a little to much Methylamine. For 100g Bromketone I added 200ml Methylamine 40%a.q. solution.
I think 160ml should be enough (after calculation 1mol Bromketone vs. 2 moles Methylamine and a little buffer for Methylamine)
experimentsciAfaik methylamine is added in quadruple excess (foolproof). It depends on the conditions. High temps, rapid stirring, open vessel, ensures a lot of it evaporates (which is not what we want).

I roughly use x 1.5

It's actually a matter of just trying and find the optimal variables as you go . There are too much for a "one size fits all".

Last Saturday did 200g batch using 400ml ethyl acetate and 400ml methylamine. That failed heavily (twice).

as I'm typing, doing another 200g batch (image). 350ml methylamine, 500ml ethyl acetate. Never fails (for me, at least).


If I would use DCM i take 600ml DCM.
 

Attachments

  • lk58qCUFHf.jpg
    lk58qCUFHf.jpg
    391.2 KB · Views: 9

TheVacuumGuy

Don't buy from me
Resident
Joined
Sep 20, 2023
Messages
58
Reaction score
16
Points
8
Afaik methylamine is added in quadruple excess (foolproof). It depends on the conditions. High temps, rapid stirring, open vessel, ensures a lot of it evaporates (which is not what we want).

I roughly use x 1.5

It's actually a matter of just trying and find the optimal variables as you go . There are too much for a "one size fits all".

Last Saturday did 200g batch using 400ml ethyl acetate and 400ml methylamine. That failed heavily (twice).

as I'm typing, doing another 200g batch (image). 350ml methylamine, 500ml ethyl acetate. Never fails (for me, at least).


If I would use DCM i take 600ml DCM.
TheVacuumGuy400g bromoketone
1000ml DCM
800ml Methylamine
39 Celsius
6 hours (unintentionally, fell asleep)
In the morning added 1000ml water.

Cws7XTDVEa
 

TheVacuumGuy

Don't buy from me
Resident
Joined
Sep 20, 2023
Messages
58
Reaction score
16
Points
8
And how much gram 4mmc u get?
$!$It finished drying to complete dryness just now. i got 265,5 gram. Could have been higher if i actually didn't forget to wash it 3 times.


Will also get losses when crystallization to account for, so finally it will end up bit lower.
 
Last edited:

TheVacuumGuy

Don't buy from me
Resident
Joined
Sep 20, 2023
Messages
58
Reaction score
16
Points
8
And how much gram 4mmc u get?
$!$i just finished reacting another one, 200g, 800ml DCM, 400ml Methylamine. ~2.5h 40 celcius.
now in freezer to prepare for acidify. curious to see if it yields more and better.
 

TheVacuumGuy

Don't buy from me
Resident
Joined
Sep 20, 2023
Messages
58
Reaction score
16
Points
8
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)
 

$!$

Don't buy from me
Resident
Joined
Jan 24, 2024
Messages
102
Reaction score
24
Points
18
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

Don't buy from me
Resident
Joined
Jan 15, 2023
Messages
345
Reaction score
155
Points
43
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
 
  • Like
Reactions: $!$

$!$

Don't buy from me
Resident
Joined
Jan 24, 2024
Messages
102
Reaction score
24
Points
18
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 ??
 

$!$

Don't buy from me
Resident
Joined
Jan 24, 2024
Messages
102
Reaction score
24
Points
18
I made much year ago on dcm
 

Attachments

  • pcLNaGhdme.jpeg
    pcLNaGhdme.jpeg
    4.7 MB · Views: 11
  • oIpfGverHa.jpeg
    oIpfGverHa.jpeg
    5 MB · Views: 47
  • Lk5wBOYXvA.jpeg
    Lk5wBOYXvA.jpeg
    5.1 MB · Views: 49

experimentsci

Don't buy from me
Resident
Joined
Dec 17, 2023
Messages
17
Reaction score
3
Points
3
I made much year ago on dcm
$!$How exacly did you worked for this? What is on last picture?
Reaction vessel is just standing in waterbath without stirring?
 
View previous replies…

$!$

Don't buy from me
Resident
Joined
Jan 24, 2024
Messages
102
Reaction score
24
Points
18

Attachments

  • vDHPcqC4Ia.jpeg
    vDHPcqC4Ia.jpeg
    223.3 KB · Views: 10

$!$

Don't buy from me
Resident
Joined
Jan 24, 2024
Messages
102
Reaction score
24
Points
18
How exacly did you worked for this? What is on last picture?
Reaction vessel is just standing in waterbath without stirring?
experimentsciis much method to made it longer shor simple hard.
I dont use anymore dcm to much work ok him.
I made form start do crystal 24h max on big scale
 

Attachments

  • tXa6uL8g1Q.jpeg
    tXa6uL8g1Q.jpeg
    7.7 MB · Views: 70
  • xWDwX61T3i.jpg
    xWDwX61T3i.jpg
    438.8 KB · Views: 11
  • Yz0oANK341.jpg
    Yz0oANK341.jpg
    274.5 KB · Views: 11
  • dGgtL56RPv.jpeg
    dGgtL56RPv.jpeg
    5.1 MB · Views: 54
  • wriXDYBzT1.jpg
    wriXDYBzT1.jpg
    251.9 KB · Views: 11

Throw-off

Don't buy from me
Member
Joined
Feb 18, 2024
Messages
43
Reaction score
17
Points
8
is much method to made it longer shor simple hard.
I dont use anymore dcm to much work ok him.
I made form start do crystal 24h max on big scale
$!$Beautiful, Your an artist.
 

experimentsci

Don't buy from me
Resident
Joined
Dec 17, 2023
Messages
17
Reaction score
3
Points
3
Aha Dzien dobry. Maly mowi po polsku :)
Would you like to tell me how you worked?
I was thinking DCM method is the best for big scales...
 

HewHiSt

Don't buy from me
Resident
Joined
Jan 19, 2024
Messages
25
Reaction score
20
Points
3
Hey how can i dissolve methylamin HCl to get methylamin 40% aq. ?
I know i need to create a base (sodium hydroxyde 25%) and after add it to the methylamin but i dont know the proportions
Anyone can help me ?
 
  • Like
Reactions: $!$

Throw-off

Don't buy from me
Member
Joined
Feb 18, 2024
Messages
43
Reaction score
17
Points
8
Hey how can i dissolve methylamin HCl to get methylamin 40% aq. ?
I know i need to create a base (sodium hydroxyde 25%) and after add it to the methylamin but i dont know the proportions
Anyone can help me ?
HewHiStLaboratory FAQ has a whole thread about Mole Ratios etc.
 

spongebomb

Don't buy from me
Resident
Joined
Nov 8, 2023
Messages
7
Reaction score
3
Points
3
one question, i cant find a answer until now.
When the temperatur is so critical, why not cooling the rmx all time long ?
maybe not more than 25°C ? Hope not too silly the question
 
  • Like
Reactions: $!$
  • 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