Question Urgent help needed

[kokkewiet]

We have so far lost about 400g in final product with the methedrone easy synthesis. . We are close to cutting our wrists as we are going to loose everything if we can't get this up and running.
The product remains burning and has a strong chemical smell and taste. I'm not sure if it could be the DMA?

This is the ingredients that we have available. Perhaps we should start there. If you can confirm for me that all ingredients are right.
2Bromo 4 (Powder)
Methylamine Hydrochloride (Powder)
Hydrochloric Acid 35%
Dychloromethane stabilized CP (C H2 C12: 84.93)
Acetone with description:

(A flammable liquid with a pungent odour free from sediment)
Acetone with description:

Pure fast acting ketone solvent
Effective at dissolving and cleaning grease, oil, fats and adhesives
Fast acting resin and paint diluent
Methanol Free
Benzine with description:

Alphatic Solvent Blend
Effective at cleaning and removing oils, fats and adhesives
Softens rubber surfaces
Methanol Free
Normal household Bicarbonate of Soda
Sodium Hydroxide Solution 1N
Sodium Hydrogen (Bi) Carbonate CP (C H Na 03: 84.01)
If we could get a step-by-step procedure. If something should be shaken with cold water, please indicate. If it should be boiled, please indicate. If it should be closed / open lid, please indicate. IF it should be in the freezer or dried somewhere, please indicate. We do not have lab equipment yet and therefore using glass bottles.

 

[HerrHaber]

Well, ghetto equipment works best for an experienced chemist... The successful way is to start with the standard lab method and then reduce the complexity of apparatus. One clear point is that you used methylamine hydrochloride and for the normal synthesis the aqueous freebase solution of 40% is what most people use, what happened is that the hydrochloric acid from the methylamine salt you used will affect the bromine from it's activated position and it will be less willing to switch places with the amine moiety, then the normal excess of freebase methylamine would have to catch the halogen ion but you already have an equilibrium from using the salt instead of freebase. I'm sad to announce you that your reaction mixture/product is unfortunately impossible to save. But I would gladly guide you in making a new batch given that your DCM and acetone have been distilled prior to use (this requires what I call a minimal chemistry set for which vevor has a good price).

 

[Osmosis Vanderwaal]

Here here

 

[HuNEPper]

I used HBr during the acidification, but it was too much (ph2-3). I was able to bring it back to 5 with baking soda solution, but there is no precipitation. Is there another solution or is it trash?

 

[Osmosis Vanderwaal]

IIt's impossible for anyone to say with no more info than this. Ifnyounhad been successful up to this point, than usually what happens when you go past your ph is a loss but not a complete loss. People are not immune to throwing away the wrong fraction or using the wrong solvent, and precipitation not occurring. Barring that younHBr'ed the wrong fraction of your solvent, I would at least reduce my rm by 50% and put I in the freezer and see if anything crystallizes ( or hiring the other solvent, which you saved if your not crazy )

 

[HuNEPper]

this was the first attempt, before that I only tried NEP.

Mephedrone Hydrobromide Synthesis

Mephedrone hydrobromide synthesis from 2-bromo-4'-methylpropiophenone with n-methylpyrrolidone.

bbgate.com

I tried to make this synthesis.
It's been in the freezer for 24 hours but no crystals.