4-MMC - Whats wrong here.

[RegulierTier]

Hey guys, I wann to make some Mephedron, but i don't get it

I solved 100g 2b4mp in I think 300 mL DCM. Then I added 150 mL Methylamine over 3 steps.
The products was washed with water and seperated.
The product was a deep orange soution.
Then I started adding a Aceton/HCl solution until the pH is 5,5.
But then noting... No mephedrone Falles out. Why not?

Last time I did shake and bake method with benzene instead of dcm and this worked.
But this time... what sm I missing

 

[Osmosis Vanderwaal]

I know nothing. Seems like you should have used 200 ml ( or g?) Of methylamine, if grams, 232 ml. That would be the stoiceometric amount. I think Depending on how much hcl you used a lot of it could be dissolved in that water.

 

[RegulierTier]

I did the weile thing again.

One time I used 500 mL DCM and solved 100g 2b4mp in a RBF. Then I gave 200 mL Methylamine 40% over time to the RM and let it react under stirring by 38°C for 2,5 hours.
Then I washed it with dH2O and collected the organic phase.
Then I gabe HCl 37% to it under Sterling until pH = 5,5 and again nothing... Only a deep brown orange solution.

2nd try I made parallel I gave 500 mL DCM to a bottle and solved 100g 2b4mp.
Then I gave 200 mL Methylamine in 50 mL steps to it and shaked it 2,5 hours.
Then I washed and so on like I did in the writeup above. And again, nothing... Why?

The last time i did exact the same but with benzene as solvent and it worked perfect.
Whats wrong here?

 

[TheCook]

Hi,

Did you keep in mind, that when using DCM the organic phase with your product is usually the lower layer and the water floating on top?

If you respect that, there a serval issues here anyway.
Frit was on the right way, but you have used way too much Methylamine.
The stoichiometric ratio of the reaction is 1:1. 1 mole of 2-bromo-4'-methylpropiophenone reacts with 1 mole of methylamine to form 1 mole of 4-MMC freebase. The quantities you have used correspond to 0.440 moles of 2b4mp to 1.931 moles of methylamine. You have used approx 4.4 times as much methylamine as was actually required.
With 100g of 2b4mp and a stoichiometric ratio of 1:1, you need 38.12 ml of methylamine 40% in water.
The use of excessive amounts of methylamine leads to serval problems, you might have to deal with now:

1. Potential of synthetic byproducts
The probability of undesirable by-products is increased. Impurities can have a massive influence on the crystallisation of the hydrochloride.

2. Disrespecting the the Nernst's distribution law
Washing 1 time with water is not sufficant,, you have to do that at least 3 times (with fresh water). Otherwise you take over a lot of impurities to your freebase. If anything crystallises, you have to wash it out with acetone afterwards. The fewer impurities in the base, the less loss of product due to the acetone wash.

If you haven't accidentally tipped your product down the toilet, you now have to deal with cleaning up the mess.
This is not only annoying, but also unnecessary extra work. Do you have a distillation apparatus to get rid of the solvents??

Regards

 

[RegulierTier]

Yes I kept the loser organic phase.
I didn't calculate how much Methylamine I need. I know that methylamine was added in excess and used the same ratio which is described in the most topics here.
Last time I used the same ratio and it worked fine.
And yes I washed it several times with water, not only one time.

 

[Osmosis Vanderwaal]

I said in a thread a few months ago that the guy used 8x the stoiciometric amount of methylamine and he responded that he followed the instructions, so I checked the synthesis on this site and it's true they do call for multiple x the balanced amount. Check them yourself and see.

 

[Osmosis Vanderwaal]

So it seems the only things left are the reaction didn't reach the required temps, didn't react long enough or were under/ over protonated by the hcl. I too have failed this synth. Twice, matter of fact, in ethyl acetate. The last time I got crystals that looked right, had the right solvency in multiple solvents, melted at the right temperature and 8s identical to the product I was making except it had 0 potency. I'm making my own methylammonium chloride and refining it. I'm at a loss. The CH³NH²HCl looks different from the ammonium chloride. Puts off flammable gas when neutralized by NaOH+ water.... I don't get it. The 2-b-4-mp burns your eyes out and nose run while smelling like orange liquor. I'm lost too

 

[experimentsci]

I also one time tried in Ethyl Acetate and the product was not strong. I don't know, but maybe the ethyl acetate reaction is not a good route?

 

[badboy345]

Brother, I'm new here but I've never heard such nonsense. Mephedrone production is like ice cream production, simple and pleasant. You can make methylamine, but not mephedrone xD. Ph has nothing to do with it, you can have ph 1 and still get 4mmc. methylamine should be 20ml 200nl 2l depends on the quantity 2b4m 10g 100g 1kg. The same applies to the solvent, the more of it there is, the more of the final product there is. There is a table from Russia about how long you should boil dcm and how long you should shake dmso. the same with water+soda cleansing a few times water and solvent extraction Acetone is not even needed only in the crystallization process. This is the production philosophy of 4mmc and 3mmc.

 

[Osmosis Vanderwaal]

Such nonsense as what? The reason I'm talking about Ph is I'm starting from methylamine HCL ( methylammonium chloride) and deprotonating it in-vitro ( well I'm trying to) methylamine is unobtainable here, I wish I could just buy it. Getting someone to mail it here is as easy and as dangerous as having crack or lsd mailed to you

 

[Berlin777]

Such an annoying attitude, I see no point mocking someone who’s looking for help. If you want to help just tell what could go wrong instead of telling your life stories like someone gives a fuck.

 

[badboy345]

Brother, I'm learning on my own from the benzene video. But from what I wrote here, you can do it perfectly, as you can see. I have already done 3 4mmc syntheses in my life. I don't know how to help if he didn't show how his synthesis works, so anyone could give him some advice.

 

[badboy345]

When i throw all acid i get it i thing is no so bad O other color only white milk

 

[badboy345]

Today i try 2 times and get the same effect.
U need te as what u do and maybe somebody can help you bro.

 

[badboy345]

I'm get ph 4.
I'm need dry liquid and tomorow i'm will say u how much gram i get.

 

[badboy345]

From 100g 2b4m but need dry tomorow send u dry powder

 

[badboy345]

It's not warm in my basement and it takes a long time to dry. It's still wet

 

[Berlin777]

You claiming that you get yield over 100% from BK4 right?

 

[Marvin "Popcorn" Sutton]

Berlin777 It's a wet product. It may still need to be cleaned. Just an intermediate weighing.

 

[Berlin777]

why doesn't he just crush it down and make thin layer for quicker solvent evaporation?

 

[badboy345]

was 146g well.
is still wet but lost now 46g.
if dry can get 75g do 60g dry powder

 

[badboy345]

4-MMC (mephedrone) synthesis. Complete video tutorial.

https://bbgate.com/threads/4-mmc-mephedrone-synthesis-complete-video-tutorial.616/

bbgate.com

All is there how to made pure powder.

 

[RegulierTier]

What's up with you? You send me your pictures via DM, then post all the pictures here again... And now? I don't understand. The question was whether someone can tell me what went wrong here because I did everything as usual, except that I substituted benzene with DCM and strangely, no product precipitated. The procedure is the same as described in almost every second topic here and also the same one you described to me, except for the solvent.
Do you have anything useful to contribute or are you just trying to show off that you didn't have any problems? We've already discussed the same thing via DM, but so far, you couldn't pinpoint a mistake in my approach... So, I'm wondering what you're trying to communicate here.

Now, back to the topic... I've been thinking again and I realized that my solvent and methylamine were both very cold, coming straight from the refrigerator when I mixed them together. I'm not sure if that could be the reason because I heated the whole thing for 2.5 hours at 38°C with stirring, and even during the shake and bake attempt, enough heat was generated in the reaction. For my next attempt, I'll make sure my 2b4m/DCM solution and methylamine are at least at room temperature before mixing them.
Otherwise, I'll have to try again with a different solvent next time.
Does anyone else have any ideas? I just can't figure it out... Apart from substituting benzene with DCM, I've done nothing differently than usual and nothing different from what's described in many places in this forum.

 

[Marvin "Popcorn" Sutton]

Many people promote their synthesis methods in PD and offer paid services. They don't create their own threads, but post in other people's threads.
In difficult situations with syntheses, you can contact forum experts in private messages for free. And we will try to help.
I sent you a message.

It is necessary to understand your actions step by step and make corrections.