4-mmc turn red. Why?

[craris100]

I always do the same procedure with DCM and today i get a red product after acidification.

100g b24m
200ml Methylamine 40%
2 hours at 38-40C
And i wash the organic phase still methylamine odour is dissapeared.

When i acidify the base with HCL i get a red-brown product.

Anybody knows whats the problem here?
Thank you


The procesure i use. Here.

4-MMC (mephedrone) synthesis. Bromination in dichlormethane.

We'll consider mephedrone (4MMC) synthesis in this article. Dichloromethane (DCM) is used as a solvent. It has a low boiling point (~40 °C) and synthesis procedures take a little time. Work conditions: Air temperature 20-24 ºC; Relative humidity

bbgate.com

 

[fidelis]

i was reading the replies to the synthesis you linked, user @CristalKing said "In my opinion ph2-3 is perfect. Product has a little to much acid but product will be more white, If ph will be about 5-6 product could be more brown" so perhaps it has something to do with the pH?

hope this helps ^_^

 

[HeavenChem]

2-3 pH ? This is crazy...
You need 1 moles of hydrochloric acid on 1 mole of 4-MMC free base
Environment is absolutely neutral, pH = 5.5 with proportions above.

Sometimes you read the advice of other people on this forum and losing your mind. What the f*ck is going on here ?

 

[Berlin777]

Too much acid or you added acid too fast

 

[craris100]

Its possible. Thank you!!
I add 300ml of acetone to the base in DCM and i add the hcl:acetone 1:3 but maybe i add too fast yes.

 

[Berlin777]

I am helping one guy out, he done exactly same methodology I do but his stuff turned red. I saw he was adding acid acetone too fast but intentionally I didn't tell him anything so he know how fucked up stuff loks like

 

[Jordan Belfort]

Freeze your aceton and HCL beforehand. should help incase of acid burning.

And put automatic high speed stirrer

 

[craris100]

Its weird because is not the first i do this synthesis but today and yesterday was the first this happen. Yesterday and today i used a different 2b4m of other supplier and i was thinking is that.

 

[craris100]

Please @$!$, im not going to pay you 5000€ and nothing for this synthesis.
Stop of offering your recipe please, im trying to help to other people too.
One month trying to sell me your shit procedure every day via Telegram, please stop.

 

[HeavenChem]

His product is over acidificated. How it can be good ?

 

[TheVacuumGuy]

Probably switched vendor recently?

Do the water washings to extremes. Everytime after washing and separating, check the water layer. Stir/shake vigourously.
Repeat!

Only stop when you would dare to drink the water layer (by clearness)

No red or green ever since.
Even on DCM, no heat, 75 minutes

 

[w2x3f5]

It’s worth measuring the melting point of your 2b4m sample, it should be about 74-77 degrees approximately. I suspect that there are impurities in your 2b4m

 

[HeavenChem]

Problem also can be in DCM if his supplier added alcohol in there. I had almost same issue. This color can't be washed with acetone or ethyl acetate. Only isopropyl alcohol helps, but with high loses

 

[DavidNichols]

Ethanol wont cause and problems. Its methylaniline byproduct from dirty precursor.

 

[HeavenChem]

IPA with acetone can give red colors

 

[4synergy]

How to fix this problem ?

 

[TheVacuumGuy]

see @w2x3f5 's answer above. or mine, another one above.

And if - As a beginner in chemistry, don't expect it to succeed instantly... prepare to waste multiple kg of bromoketone on failures before you understand what is going on, and good things happen.

Oh , almost forgot. Don't let color fool you (unless it is real deep green paint like shit).

 

[chudakrekt]

When acidifying, the temperature should not exceed 30*C, if up - place in water
Use mixer speed 180-250
Use isopropyl alcohol to add acid After you have reached Ph 5-5.5, you can evaporate a quarter of the liquid and put it in the freezer, thereby skipping the step of obtaining flour and immediately getting crystals
I have created more than 600 kg of this substance, I think I will write manuals for this forum in which I will tell about all the possible mistakes of beginners, show all the tricks and possible synthesis options

 

[TheVacuumGuy]

Please enlighten me. Why would one add more acid when ph target reached?

 

[chudakrekt]

Add more acid to get more product
But it will need to be set at a lower temperature.
When acidified to Ph 2-3, the meph becomes more stimulating, but does not lose the power of euphoria

 

[chudakrekt]

Next week i post thread with sinthes

 

[HeavenChem]

Did you knew what 2-3pH resulting degradation of 4-MMC ?

 

[TheVacuumGuy]

Still waiting

 

[HeavenChem]

Lol, metal mixer on acidification process ? Sounds like grey color failure on finish

 

[HeavenChem]

Problem can be in local over-acidification.
When you adding acid too fast your 4-MMC turns in to shit.
Place your beaker on ice bath with magnet stirrer and under separation funnel. Reaction temperature should be not more than 25-30 degrees Celsius. Use about 2-3 drops of concentrated hydrochloric acid per second on 1000g of bromoketone-4
Also red color can be from alcohol in reaction mass. Make sure what your DCM is pure.

 

[chudakrekt]

About the speed of adding is true, but there are methods with very fast moving You can also use hydrochloric acid IPA

 

[HeavenChem]

In that case you should not use acetone. I don't like IPA methods anyway