Biggest mmc problem! Blue product

Rush-Benzo

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Is there any way to clean such powder of different colours (blue, red) afterwards? Rinsing with cold or boiling in hot acetone will not help.
 

TheVacuumGuy

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I found ethanol to work perfectly for getting rid of green/blue
 

G.Patton

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Methylamine excess can give such color. You have to be sure that you have got rid of methylamine after reaction before acidification.
 
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w2x3f5

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Do you know why methylamine can produce colored impurities? I have seen many samples of white mephedrone laced with methylamine without a hint of staining.
 

G.Patton

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Probably it is combination of several factors. I can't say for sure.
 

w2x3f5

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I'll try to somehow specially make a pair of separation of the amine ketone salt from a solution with an admixture of methylamine. 5 people contacted me, in all cases the culprit was bromketone.
 

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Once I have several kilos of dirty flour, how do I try to get rid of this methylamine?
 
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Chemix-Express

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Yes. But when such coloured powder is dissolved in various combinations of water and acetone, a butter or such oatmeal comes out, which becomes coloured again during filtration.
 

w2x3f5

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The admixture of methylamine did not give color to the solution and powder when the acid was added. I checked the mixture of dichloromethane, free base + methylamine impurity, the mixture after amination, the aqueous methylamine layer was discarded, the dichloromethane layer, on purpose, was not washed with water. The addition of hydrochloric acid to dichloromethane did not give color, the powder fell out immediately and was almost white (slight yellowish tint). If necessary, I can provide more detailed information on experience with photos.
 

G.Patton

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Thanks for your research! It is valuable information. Could you please add some pictures here?
 

w2x3f5

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left photo after addition of acid to dichloromethane with free base and methylamine impurity (specially). right photo end of methylamination, before separation of the aqueous layer of methylamine
 

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mocnykutas

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Whis what u need get when u throw acid HCl
 

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zbro

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If the contaminant is a condensation product of amino ketone and 4-methylpropiophenone, then these are heterocyclic compounds of pyrazine (they are not ketones). The amino ketone can be purified using a bisulfite adduct, provided that there is no other ketone in the mixture, i.e. 4-methylpropiophenone. Cyclic ketones add sodium bisulfite, giving a salt of a-hydroxysulfonic acid, which is insoluble in organic solvents but more or less soluble in water. Pyrazines do not react with sodium bisulfite. Adding sodium bisulfite solution to the contaminated mixture will produce an adduct, the latter is a solid, this adduct can be filtered off and then it can be decomposed under the action of acids or bases, recovering the starting ketone. Sodium bisulfite reactions are used to purify BMK from mixtures with other organic compounds.
 
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