Cristalização da mefedrona (4MMC)

[William D.]

Não há cristalização em DCM. Apenas água+álcool (vodka), água+acetona. Proporções - 1:1 - 1:3 pó:líquido. A percentagem de acetona/álcool em água depende da qualidade e pureza do pó: quanto mais sujo, mais. A taxa de crescimento e o tamanho dos cristais dependem da quantidade total de solvente

 

[Ranbir Singh]

Which solvent is best in making and crystallization please tell me sir

 

[ghostimage]

i have a questions about crystallization of 4mmc*hbr(!! not hcl) so i used to work with scales about 15kg in one pot
my yields in bromination is 96-100% of theory, amination give me 86% of FB (it is theory almost max, you cant move further balance of reaction) and acidification with
diluted hbr in totalness to make 1g mmc to 2.5ml o water. So, even without washing i have this after acidification -

clean,needles matt like fiber glass (room temp +8) but allexcess water inside this matt, and this is problem.First time i try to melt it, place in +22c 35% humidity, and after 4 days i have this -

some are okay, some not. So the problem is something inside is oxidizing or simple condensed to trash point where it osibviously bad.
DCM is bad in washing aquos solution of 4mmc, he only wash some trash which is nonpolar. So it can help but a very little.
My question is - how to extract clean 4mmcHbr fron not so clean brine h2o.
First i thought. thay if a lot of mmc precipitated at +8c, maybe it`s much more simple in comparison with 4mmcHcl to make a cold extraction, so i try 500ml h2o +40g mmc, and place in friedge for 12h, no result, how is it?!

overall i have a few ways - try salt\acetone extraction
try to crush this glass like matt and rinse with ipa\acetone
or ...a lof of or.... So i need a man with expirience with 4mmc*Hbr (i`m a pro on hcl, but this situation is slightly different)
on all photos here - same mef in h2o, and sorry for my eng

 

[loadingST]

Wow, i havent tried to make hbr cathinones, its one of my intends to try out some hbr salts too,it seems its less soluble then hcl in water ?, i usualy get donations from guys with almost exact the same peoblem but with hcl, i know how to remove yellow collor and then crystalize into transparent glass, as hbr is more bulky it makes the mass of pure product wven more, in this moment im rhinking did anyone ever tried to prepare a something with HI acid xd

 

[ghostimage]

at first i think that graph temp\so;utability is moved far right in comparison with hcl, like hlc mmc crystallise from water at ~ -18c, but now i make a test and seems that no, it`s no temp\solutability, it`s about overall solutability in water, as you say.
I know too, but i need a dessalination\freezeng parameters with precise, i need 100% yields, without any product in the trash. btw i make 4mmc for 3-4 years in scales from 15kg to 150kg in onepot, but i reach the point, than my russian\ukranian community cant effectively find solutions for this small problems,and i try bbgate cause in overall 4mmc synthesis is easy as crap, but details....details are the devil in the box)

 

[ghostimage]

like, for mmc*hcl you need to cool solution with 1c at hour from 25-30 to -18 if you use nacl\acetone\ethanol etc, so mmc*hcl percicipate almost fully, maybe 2% lost in solution, but for mmc*hbr no one can realy answer me

 

[ghostimage]

HI no, its toxic, the most easyiest form of salt for human biochemical is orthophosforic acid (in east europe used for soldering) cause phoshates is energy cycle of human, like ATF etc, but cons are - even less time duration, pros - weight even more than hbr and compeletely legal to buy.
damn, i even one time try to lemon acid from your local food shop, it`s works but in help with microwave owen, some funny shit the porcuct is mefedrone citrate, crystallize from gummy like squish

 

[loadingST]

Haha nice to meet guys like you here, i havent done anything large never, im just a hobby chemist, for crystalization i use the slower way always i hadnt had to rush for anything, but realy you method is a lot less time consuming and a lot less smelly, im thinking as wee see on the image posted the crystals that form are this small icy crystals, like from very fast recrystalization, i think you had to try with more solvent and slower precipitating, maybe drop the temp by 1C per a few hours and absolutely no vibrations and free of trash inside(better filtered) and you shoud grow these bigger shards with hbr, i dont see a reason to dont.

 

[ghostimage]

1c per hour is a basic knowledge, problem is - you need to carefully control it, or use very large batch so it naturally will cool at a small pace, i will try it of course

 

[loadingST]

Yea cobtroling the temp in the room, which reflects the temp of the solution is not so basic knowledge but if you say haha, if you have time, why dont you use ipa/water for making caths crystals, yes its slow but works very clean and makes these bog crystals users want.

 

[ghostimage]

i use ipa\water, why you think i`m not? just it`s not optimal for not clean solutions.
i`m from russian side of darknet, here is 7th grader know how to make 4mmc in bottle of cola, and a lot of things are basic knowledge, not sarcasm, btw a lot of methods here just a translation from russian, and recepies is old and considered trash now. In some methods which a read here a very bad mistaces about h2o2 amount, they calculated it as br2 instead ob just br, and no extra added, so x2 +30% on top and you have 750 ml h2o2 instead of 260 or something....

 

[loadingST]

Xd i know how to calculate, 7th generation in making mephedrone aounds funny, there is just a simple machanism once you understand it it works wonders, and there is a magic trick to remove the yellow color of the solution afther dissolving meph, and whem letting it crystalize it dont become yellow

 

[ghostimage]

or you can make it clean from the start, and no any trace of yellow and no need in antioxidants

 

[Dr. MMX]

@ghostimage what is the problem on larger amounts? I suppose its need to see in the background of it. If methylamine aq is used its large amount of water which protonates 2b4m. The synthesis of 2b4m need to be careful as well, the basic informations about reagents used for nucleophilic substitution Bromine to the ring do matter. If we do not know the % of 4 mp in the 4mp we actually cant calculate it for the reaction, di-bromine will be present in case of excess bromine in the reaction, which will affect futher reaction very deeply.

I assume you used DCM for the reaction?
DCm is to be used t o extract aquenous layer from methylamine if such is used so, not to do anything after it was acid put in.
mephedrone has low solubility in DCM, it can be easly extracted by H2O and futher then distilled under pressure.

But honestly I didnt understand the problem. Is your goal to convert this salt to solvent and recrystalise? You mention extraction, I suppose liquid liquid, but cant see any, it already started to crystalise. H2O which you used in the acidification should be added more to not let salts appear during it, it lead to impurities.

EDIT I see t he question sorry
you could try to see temperature and melt the 4mmc or find the solvents which will work well for both of them and then extract again and distill under pressure

 

[ghostimage]

i know all about synthesis of 4mmc etc, what i dont know - graphs of solutability in water\temp, anything except this - is no new for me.
and, 4mmc hbr have higher solutability in dcm then 4mmc*hcl, just for info. Dcm is not so polar as benzene, and hbr molecule make the final product slightly more soluble in dcm than 4mmc*hcl because it`s very close to ketone, which we use in start. My english is not good, but thats it.

again - all i need, a GRAPH, or at least exact temp, at which all 4mmc*hbr percipitate from h2o, there is one, i ask a lot of \bright\ brains in this forum, and all i see - advice how to do that and lace my shoes, i`m not a karen, but..... if anyone dont know the answer, just say it in plain text, sorry if i sounds like karen.

 

[ghostimage]

"di-bromine will be present in case of excess bromine in the reaction, which will affect futher reaction very deeply"
do you have real expirience of that or seen a sample test in chromotograph? i always hear about enamins/over bromation etc etc, and nope, everything always okay, and purity is 94 - 97%, that is no good is cold amination, which i read here a lot of guides. like 24h....shiiit, this is real fucked up, pyrazines surely exist, moreover -

 

[Dr. MMX]

You do have a specific case, nobody will have an answear for it probably
You need to check it yourself

So it was the crystalisation problem in the beggining that you were not satisfied with its looking on the evaporating the h2o?


It was not low amount so i suppose this situation is the result of the Hbr reaction with the residues from unwanted parts what was left from 2b4m reaction. 96-100% yield is actually very huge difference, under consideration is needed to be taken the part what is actual 2b4m and residues depending on the process you performed.

I think distillation the solvent under negative pressure is the solution in any case when its mmc h2o

To get mmc from this its column needed

But to get some mass containing other things than mmc but looking nice I could try to melt it to separate from NaCl then gradual temperature reduction on overasaturated solution of h2o, the product should leave at temp could bne 30 could be 40c.

I once did Hbr, using 2b4m from " shop" with unknown procedure. The result after evaporation under pressure of h2o mmc hbr was a little " yellow". So it was only thing to do. In the h2o I think it little yellow was good looking at 40c or so... resulting 50% of the mass, not sure.

 

[Dr. MMX]

You do have a specific case, nobody will have an answear for it probably
You need to check it yourself

So it was the crystalisation problem in the beggining that you were not satisfied with its looking on the evaporating the h2o?


It was not low amount so i suppose this situation is the result of the Hbr reaction with the residues from unwanted parts what was left from 2b4m reaction. 96-100% yield is actually very huge difference, under consideration is needed to be taken the part what is actual 2b4m and residues depending on the process you performed.

I think distillation the solvent under negative pressure is the solution in any case when its mmc h2o

To get mmc from this its column needed

But to get some mass containing other things than mmc but looking nice I could try to melt it to separate from NaCl then gradual temperature reduction on overasaturated solution of h2o, the product should leave at temp could bne 30 could be 40c.
But its to be tested on the small amount and just see the result if it fits

I once did Hbr, using 2b4m from " shop" with unknown procedure. The result after evaporation under pressure of h2o mmc hbr was a little " yellow". So it was only thing to do. In the h2o I think it little yellow was good looking at 40c or so... resulting 50% of the mass, not sure.

As well the waiting till h2o evaporates is not very optimal choice, however if grams do matter it probably is, but I would not take it as a final yield. crystalisation is final purification process.

 

[Dr. MMX]

even usage of methylamine aq already does affect the reaction with the 2b4m because of the water

Excess bromine is excess bromine... In the reaction we do need exact amounts, thats why technical data of the 4mp is needed to prepare it well for the futher reaction. It does not just disappear if its overdosed.

the "cold amination"

Methylamine may be used in liquid directly, it will probably solve the problem of the water and its negative impact. I will share the result of the tests

If hbr was used a lot of things matter more than hcl was used, maybe thats why it was not noticed any difference. WIth KBr it just reacts futher more with the already put water + 2b4m and its residues

 

[Dr. MMX]

24 grams in 120 ml of h2o2 appared as a salt at 2c, thats the infromation I can supply you with