Mephedrone (4-MMC) Synthesis [2B4M, Ethyl Acetate, Methylamine HCl]

[c01db100d_india_mephedron]

Can we replace

MA HCI to
METHYLAMINE (mono) 40%
CAS.No: 74-89-5

Ordered

2-Bromo-4-methylpropiophenone 1451-82-7
Acetate
NaOH
Acetone


Tell me if we need something more ?

 

[PlayTag]

Do you have any info on how it's made with methylamine aq40%

 

[handle]

Awesome, thank you for sharing this.
In step 6. Add methylamine HCL into flask Am i adding the methylamine HCl crystals? crystal / powder form?
Just thought id double check this first before i attempt.
Thanks again

 

[Dr. MMX]

Yes. You need to have flask with reaction and beaker with naoh water at room temp and methylamine hcl measured to be put in

Yes, methylamine hcl is in powder/crystals form.

 

[handle]

Thank you. sometimes reading all the posts can make things more confusing. ill try your method here first.
Try and keep it as simple as it is.

 

[Dr. MMX]

Its advized to read the whole process until every step is undersood. Its good practice - planning. If something goes wrong (if you will be confused during the process you may risk its success). If you do understand each step what to do it incrashes your chances for success

as well reading the book "lab techniques for begginers" contains priceless informations (I uploaded it into library)

 

[CARLITOBRO]

Anyway i have some questions here if you dont mind and thank you in advance

1. Used 20gr of bk4 in 100ml ethyl acetate in 500ml round bottom flask reflux attached in a water bath 40c-60c waited till all bk4 dissolved and temp reached 50c in the water bath added at once 100ml of 40%aq methylamine let it reflux for 45min and added 150ml of water and separate the organic ( by the way it was so poor yield not even 10ml yellow oil).

2.Removed while still a bit hot added 20ml ice cold acetone and begin adding 33% hcl drop by drop the solution becomes RED and quicly turned green

1.WHAT AM I DOING WRONG there is no color change after adding methyl 40%aq with stirring it just goes from opaque to yellow after 30min

2.when using ethyl acetate and methylamine aq 40% is it better to heat up with stirring OR the opposite cool it with water bath and keep to reaction cool ?

3.before acidification and ice cold acetone adding to the organic solution is it better to cool the organic phase after separating in the fridge or just added the ice cold acetone ?

 

[handle]

I read the instructions and its quite clearly states:
3. After 2b4m is dissolved, put dish with cold water, to provide cooling to flask

 

[Dr. MMX]

Hello,
1. IT seems to be a little too much of methylamine, but I dont think it could cause anything wrong at all in such scale. Your paramets seems to be ok... maybe there was too much delay between processes? it decomposes very fast.
2. it cant be hot, its advized to be cooled before
1.1 Not sure

2.1 For such scale no heating is needed, cooling as well, but i d like to strart at 40c becasue its better for reaction (for such scale)

3. yes it is, but you do that using ice bath and stirr it inside.

 

[CARLITOBRO]

thank you and i tweaked like you said ..heating to 40c and cooling before acidification and also one major thing also is reaction time downed to 20min AND THANKS GOT A YIELD OF APROX 60%. thanx bro...

 

[ghostimage]

you need at max 50ml of dissolver, on such small scale, even less
you need 20ml of aq MA
you dont properly wash out excess of MA, add acetone and THAN hcl, so you 1 - produce a lot of enamines and 2 - your hcl goes to leftover MA. And i dont know temp scale for EA, i always use dcm, and for dcm 36 is border line and boiling is complete disaster.

 

[CARLITOBRO]

thank you very helpfull i will tweak again and replay with the results

 

[siko]

hello
9. Sodium bicarbonate 5% H2O solution 300 ml was poured into flask with freebase then stirred for 30 mins. After that layers are
how much Sodium bicarbonate do you put in the recipe?

 

[Dr. MMX]

5% Nahco3 in h2o means 285 grams H2O and 15g of NaHCO3 (sodium bicarbonate)

 

[siko]

hello i am new are i have no experience , i hope will have it later thanks.

 

[ghostimage]

you must not use soda on any step of 4mmc, it is produce more problems than solutions, all you need is wash wash wash.
bromination ccan be done with 100% yields with clean result, amination...yes, only 3-5x waterwash, acidation, again, can be done clean way, but at least one wash is must.

 

[ghostimage]

this is my bromination, it is so clean, that crystalls of bk4 not appear even at +33, you need to touch supercritical fluidand in 5 secall is crystall, or you can add cold water realy fast, but in the process it is drops some crystals if temp lower than 65, which means there are not centers for crystallization in the end, but in the middle of process, sry for my eng btw.

 

[Dr. MMX]

Sorry I dont understand its information. Is it about nuclephilic substitution of bromine into the ring?

 

[siko]

me too not understand sorry

 

[ghostimage]

yep, in my case h2o2+hbr+hcl(small quantities for calatyst) + 4mpf

 

[siko]

hello if you are already sharing why you don't write down the process what needs to be done from 1
with all the numbers and quantities.

 

[ghostimage]

1L of 4mpf + 850-900ml 48%hbr + 45ml 37% hcl + 700ml or more h2o2(drop by drop on 75c), without cooling it`s 85 minutes at 10c roomtemp, after the process stirr another 30 min, if you have excess brom in water - it will react on complex chain and discolor to water solubale acids etc, than just rinse br4 crystall with water, it must be no acid - (ph around 8-9) you will get in max 1532g of bk4.
i dont share cause i dont know what is crucial information on this forum, if you have questions - i ask as far as i can, i`m not a chemist by degree, just a lot of experiments and obtained knowledge

 

[siko]

hello Dr. MMX do you know where i can buy methytlamine hcl

​

 

[Dr. MMX]

Most often purity of 4 methylopropiophenone is 95%, we should know the exact data but if we cant, we use 95%, so for 1 mole of 4 methylopropiophenone we do use one mole of hbr.

4′-methylpropiophenone (CAS 5337-93-9) 1000 g
. Hydrobromic acid 48% aq . 1155 g or 775 ml. Hydrogen peroxide
(H2O2) 35% 980g, (plus 20-30% excess.
H2O2 will decompose during the reaction)
Sodium bicarbonate (NaHCO3) 595.5g,
Distilled water.
Glacial acetic acid 432ml


1. 1000g of 4'-methylprophiophenone is added to the flask.
2. Hydrobromic acid (HBr) 1155 g or 775 ml 48% is poured into the flask and stirred for 5 min. Temperature set to 60c using a water bath.
3. Hydrogen peroxide 35% 1200g is added to the drip funnel.
4. Glacial acetic acid is added through the cooler, wait until it stops "dripping".
5. H2O2 is added in small amounts. Orange/red bromine is released. When the reaction slows down we add acetic acid in small amount, equal to the total amount to be used of h2o2
6. Repeat the steps until you add 50% h2o2.
7. The temperature of the reaction mixture must be increased to 70-75c, after increasing the temperature, the addition of h2o2 and acetic acid can continue.
9. After adding all the reagents, stir at 70-75c for an hour. 10. As a result of lowering the temperature, 2b4m is formed.

Glacial acetic acid is neutralised with equal amount of nahco3 in water.


For futher reaction 90% of purity is starting data.

 

[siko]

not understand sorry what do you get from this ? 4-mmc or 2b4m

​

 

[ghostimage]

bk4 - 2b4m, i point to this in the end