Failed 4mmc synthesis

[abis777]

So, I tried yesterday my first synthesis for 4 mmc and I failed. First I dissolved 50g 2b4m in 250 ml EA Then I addead 100 ml NaOH + H2O solution and 75 g Methylamine HCL and stirred for 30 minutes. Temp raised up to 45 C after some time. After 30 min stirring (pic 1) I separate freebase from solid compounds through funnel (I get a dark brown solution on top and yellowish bottom) than I add 150 ml 5% sodium bicarbonate + H2O to freebase and stir for 30 minutes (pic 2) (the temp of RM cools down to 25C). After 30 min stirring I pour the RM in separation funnel and I rinse once with 300ml H2O (too much and maybe I should ve filtered the RM first as it was) but the layers don't separate clearly (pic 3). I wait like 10 min than separate as it is and do 2 more washes with 150 ml H2O (this time the separation is way more clear). After washes I get like 100 ml freebase. After that I add 1;1 acetone 100ml then I let acid hcl 32% drop one drop a sec and the rm gets very dark instantly (pic 4) and ph stays 0 for a long time then I throw out the shitty synthesis I made. What are my mistakes?

 

[NeoTolls]

Shit chemicals

 

[UltraHQ]

Swap the acetone for water, then add the acid and aim for ph5

This will help stop that colour change, also after doing acidification there may be left over oil, don't throw away the oil (freebase), put it in the freezer for until -15 to -18, there will be more 4mmc powder form, collect it, dry it, then dissolve in water ready for crystallisation

 

[dnBQByvHb8Zkawbjpx]

Mephedrone hydrochloride is soluble in water. When you swap acetone for water, how do you prevent 4-MMC.HCl dissolving in water and losing the product during filtration? Does freezing the liquid after filtration (which is a mixture of solvent used for the initial reaction with water) crash out the precipitate so it can be filtered again?

 

[UltraHQ]

This method is slightly different, sorry I should have explained further.

The 4mmc will now be in the water like you say, thus skipping the step where you wash the 4mmc powder with acetone after it precipitates in the acetone, the water method you don't have to wash the powder, it's in the water and you place in a controlled room temperature environment until crystalised. Or if you want to wash the 4mmc with acetone you can evaporate the water through gently boiling away the water, eventually the 4mmc powder will come out of the water, it may be a bit dark, depends on how dark your oil / freebase was to start with. Once you've boiled the water off the powder will be there but it will be very hard-ish chunks and then you add acetone to wash it whilst the 4mmc is still hot from the boiling, then mash the 4mmc chunks so it mixes amongst the acetone and then remove the acetone via buchner funnel and flask, add more acetone to further clean.

This way is a method I created myself due to not having the correct working space, so I had to come up with a way to suit my working environment and this works, I've made 100's of KG with it, it's just a very unique / odd way if you haven't done it before.

End product was always very good and we're told its the best they have had etc.

Hope that kind of helps.

 

[NeoTolls]

A lot work u say about acid and water where u take out water from freebase and all mmc is in water a lot smell and time to made it on big scale

 

[dnBQByvHb8Zkawbjpx]

Interesting, thank you for the explanation. I've always wondered what people meant by doing the acidification in aqueous environment without using acetone.

If I understood you correctly, you dilute the free base with some water, perform the acidification based strictly on pH (do you aim for 5.5 as is advised when using acetone?) because 4-MMC.HCl does not precipitate in this environment. The mix still contains the original solvent in which free base entered the acidification, so I guess you let layers separate and remove the solvent, keeping only the water layer that contains our product. Then you dry the aqueous layer, either through boiling (in vacuum would be nice) or through evaporation, to produce powder, or you consider this as crystallization and allow crystals to grow over time.

This technique would require minimum amounts of acetone, close to none, only little to wash crystals when needed.

Am I getting all details right? Please correct any wrong statement above, I'd really like to understand this in detail before I try it out myself.

 

[dnBQByvHb8Zkawbjpx]

My attempts at 4mmc synthesis have been plagued with a similar problem - during acidification, after adding just few drops of HCl, the mixture turns black. Well, black is not precise, it's either green or blue. But so dark that it appears black. Only after diluting the liquid by a large factor you can see the actual color. After adding more HCl the mixture reaches pH 5 (approximately) and the 4-MMC.HCl precipitates. Some product can be usually salvaged but it takes a lot of time and acetone to wash as much color from the precipitate as possible, and then repeatedly recrystallize and wash the crystals with more acetone to purify the product. I attach two photos from two batches to show what the problem looks like.

I always pay close attention during the flushing of free base and the resulting organic layer is free of any smell of methylamine. In my last attempt I tried to super-cool everything entering the acidification step: the HCl, the free base, the acetone, everything was freezer-cold at -18 °C, but the free base diluted by acetone turned black with about the fifth drop of HCl.

My suspicion that there is unreacted bk4 in the free base and I will focus on fixing this in my next attempt. I welcome any advice in what I can try and focus on that would explain my past problems.

 

[abis777]

so a longer reaction might do it?

 

[abis777]

What do you think is the reason the ph of solution didn't change from 0? It wasn't enough acid?

 

[dnBQByvHb8Zkawbjpx]

How do you measure pH? This sounds like an error in measurement to me. The free base starts as alkaline or close to neutral. As you add more HCl the pH slowly gets through 6 to about 5 and the 4-MMC.HCl precipitates. Getting the mixture to pH 0 sounds almost impossible to me. You'd need to dump a huge excess of acid into it.

 

[NeoTolls]

Is no problem pH can have pH 1 and u still get product but will be brown

 

[abis777]

with ph strips. I dropped a bit of acid at some point maybe that was the cause

 

[NeoTolls]

Ph2

 

[Dr. MMX]

here we do see impuirities that are the result of improper technique earlier, it shouldnt be blacjk when acidified and left out of freezer

probably its some of reaction problems, bad acetone quality, or not proper quality of 2b4m

simply test at least melting point of of 2b4m.

 

[dnBQByvHb8Zkawbjpx]

My acetone is top notch, I stand by it. However, these photos come from batches cooked with very improvised equipment - no external heat and only a very weak magnetic stirrer. It is quite likely that I ended the reaction too early given its temperature and there was unreacted bk4 left in the RM.

The bk4 itself was not of the highest quality possible but it was not terrible to be the cause of the colored mess shown above. With some upgraded equipment I was able to run a full reaction (in EA, heated to 50-55 °C, total 30 min) and the acidification finally worked as expected - I got nice white precipitate and no change of color of the RM. Below photo is filtration after acidification. The color of the separated liquid is clear and bright (previously it was all black) and the paste is almost snow-white.

Sadly, the last batch used all my remaining bk4 so I'm unable to test it anymore. But the success of the last batch confirms to me that the problem was not in my bk4.

 

[PersonVPN]

Forget about EA!!!
Very unstable method of synthesis!!!
Very difficult to isolate the final product!
A lot of losses with EA!!!
Use Xylene, Benzene or DСM.!!!
In all other respects, stick to the same recipe as described here!!
If you are just a student, do not dilute HCL acid with acetone!
It will take some time before you understand this whole process.


For 100 g of BK4, add 500 g of the solvents I indicated.
For 100 g of BK4, add all the methylamine at once. (140 ml of 40% solution in water) With large volumes, 500 g or more, add in portions and cool!


Carry out the acidification very slowly!!! up to pH 5.5-6.
Filter, dry, ( After this, rub the dry powder through a metal sieve) and only then wash the dry powder first with xylene or Benzene!! ( NO DCM !!!) and then with chemically pure acetone.

Well, when you already know all your mistakes and gain experience, you can change the synthesis conditions as you wish!

I wish you all good luck in your studies.!!!

 

[NeoTolls]

How much kg you made mmc ??
What bulshit you say dcm need heat 2h 40°c
Benzen 60°c 2h
what EA is xD
Very good is easy work only need mix 2h no like the say 30min then get more product.
Is very good method with methyloamine hcl and naoh if somebody made mistake with synthesis then is problem or 1 form chemiclas is shit Simple

 

[WalterFan]

I do this synthesis since September, everyday, I was never failed with EA even before I wrote this comment an hour ago, I finish another patch, what do you mean ? Benzene and dcm is bs when he using MA. HCI

 

[Dr. MMX]

PersonVPN
I honestly do not agree, this solvent is suitable and has some of pros - it can be recycled during sysntheiss and even its required to distill it under negative pressure
in my opinion it provides less impurities than DCM

 

[abis777]

I did a new synthesis today with way better results but I made mistakes with acidification. All things went well except at the acidification I got ph 1 and got a white solution (last picture) then I put it in the freezer. Should I continue to extract the meph tomorrow or the synth is dead?

 

[Dr. MMX]

If your caculations are correct, yoou dont need to measure ph... juist calculate molar mass of anything you do.

 

[NeoTolls]

About 110ml to 130ml acid HCl 37%if use 100g 2b4m

 

[dnBQByvHb8Zkawbjpx]

That does not sound right. It's too much, in fact it's more than three times the required amount per my calculation. Double check your work.

I calculated I'd need 52 g of HCl 31 % for 100 g 2b4m. The density of HCl 31 % is slightly higher than that of water (1.15), so 52 g is 45 ml. Your HCl is higher concentration and so you are going to need to use less of it. Roughly 38 ml, if my calculation is correct. A quick look at The simplest recipe for crystal Mephedrone suggests that I am right. The reference recipe for 100 g 2b4m uses 40 ml of hydrochloric acid (presumably maximum concentration 37 %).

 

[abis777]

how much water to add in order to be able to measure ph and not dissolve the mephedrone?

 

[Dr. MMX]

just to make it wet

 

[abis777]

wet got it

 

[abis777]

Why do I fuck up the acidification?

 

[Dr. MMX]

h2o NAoh must be prepared earlier beecasue of exothermic reaction, it must be chilled 1st then addded


thats for 1st