Biggest mmc problem! Blue product

[Studenttt]

Hello,
i have read that a lot off people have the problem that there mmc turns blue after adification. Why is this?

 

[Acidosis]

Hello,
i have read that a lot off people have the problem that there mmc turns blue after adification. Why is this?

Studentttthis happens when your bromine or iodine ketone has not fully reacted, surely some adjustment in the temperature or perhaps the reaction time will solve the problem, I can also advise you that when you start dripping your Hcl-acetone solution (1:5 ) keep these well cold before using and also try to put your beaker with your MMC base inside a bucket with crushed ice to always keep the base very cold since when adding the hcl the temperature rises drastically and it could also be one of the factors that turn your cat blue.

 

[Rush-Benzo]

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.

 

[mocnykutas]

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.

Rush-BenzoOnly acetone help. And use pure hcl 35%-38% no 30%

 

[Chemix-Express]

Only acetone help. And use pure hcl 35%-38% no 30%

mocnykutasI already have mephedrone salt, but it is blue-red and even huge amounts of acetone refuse to flush the colour to pure white.

 

[mocnykutas]

I already have mephedrone salt, but it is blue-red and even huge amounts of acetone refuse to flush the colour to pure white.

Chemix-ExpressChange acid hcl next time

 

[mocnykutas]

I already have mephedrone salt, but it is blue-red and even huge amounts of acetone refuse to flush the colour to pure white.

Chemix-ExpressMade crystal and later wash IT with acetone

 

[Chemix-Express]

Made crystal and later wash IT with acetone

mocnykutasNo crystal wants to grow out of such highly coloured powder

 

[TheVacuumGuy]

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.

Rush-BenzoI found ethanol to work perfectly for getting rid of green/blue

 

[Studenttt]

Yes i also think acid hcl is the problem, i have order new hcl and try again!

 

[w2x3f5]

Yes i also think acid hcl is the problem, i have order new hcl and try again!

StudentttNo, its problem only with bromketone

 

[Chemix-Express]

What the problem was is no longer important. I have a lot of coloured 4MMC powder and I can't crystallise it because of this. I am therefore looking for a way to get rid of the impurities.


Is dissolving such coloured 4MMC hydrochloride in hot DCM, successively add an equal volume of water. Treat this with hydrochloric acid (here to what PH is best to acidify so that all the 4MMC goes into the aqueous phase and the impurities stay in the DCM. PH 4 or lower?)

Subsequently separate the layers and evaporate the aqueous layer, a white powder of 4MMC should remain.

 

[w2x3f5]

What the problem was is no longer important. I have a lot of coloured 4MMC powder and I can't crystallise it because of this. I am therefore looking for a way to get rid of the impurities.


Is dissolving such coloured 4MMC hydrochloride in hot DCM, successively add an equal volume of water. Treat this with hydrochloric acid (here to what PH is best to acidify so that all the 4MMC goes into the aqueous phase and the impurities stay in the DCM. PH 4 or lower?)

Subsequently separate the layers and evaporate the aqueous layer, a white powder of 4MMC should remain.

Chemix-ExpressThe impurity is a condensation product of aminoketone and 4-methylpropiophenone, the problem is that the impurity travels from layer to layer along with the aminoketone.

 

[Chemix-Express]

The impurity is a condensation product of aminoketone and 4-methylpropiophenone, the problem is that the impurity travels from layer to layer along with the aminoketone.

w2x3f5I can't do anything about it anymore?

 

[w2x3f5]

I can't do anything about it anymore?

Chemix-Expresshonestly, it's hard. it's easier for me to make pure bromketone than to mess with dirty amine.
perhaps multiple recrystallization, or run through a chromatographic column, there are many options.

 

[Studenttt]

I think that wil not work because the colour is like paint and also will go in the water layer

 

[Chemix-Express]

So there is nothing more I can do about it I understand, or does anyone else have any ideas?

 

[w2x3f5]

Can be distilled in very low vacuum. less than 10 microns.
The second option is to select an acid and an organic solvent so that the impurity salt dissolves well in solvents, but the mephedrone salt does not.

 

[Chemix-Express]

Can be distilled in very low vacuum. less than 10 microns.
The second option is to select an acid and an organic solvent so that the impurity salt dissolves well in solvents, but the mephedrone salt does not.

w2x3f5Currently, the last thing I can think of is to dissolve 1g of dirty 4MMC in 1ml of hot water. Let's assume that we then have 500ml of such a solution. So we then add 250ml of DCM, stir vigorously after which the aqueous layer once separated goes to crystallise.

I guess the last hope in this

 

[w2x3f5]

Currently, the last thing I can think of is to dissolve 1g of dirty 4MMC in 1ml of hot water. Let's assume that we then have 500ml of such a solution. So we then add 250ml of DCM, stir vigorously after which the aqueous layer once separated goes to crystallise.

I guess the last hope in this

Chemix-ExpressI'd rather try boiling the salt in dichloromethane, without water, perhaps periodically changing dichloromethane to fresh. it is necessary to control the coloring of dichloromethane, if the color does not go into dichloromethane, then there is little point. you can try acetone. it's all perversion

 

[G.Patton]

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

 

[Chemix-Express]

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

G.PattonOnce I have several kilos of dirty flour, how do I try to get rid of this methylamine?

 

[Chemix-Express]

try to use Isopropyl alcohol (IPA) or ethanol

G.PattonHow much IPA per 1g of flour do you suggest?

 

[G.Patton]

How much IPA per 1g of flour do you suggest?

Chemix-ExpressRead about it here.
Mephedrone (4MMC) crystallization

 

[w2x3f5]

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

G.PattonThe 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]

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.

w2x3f5Thanks for your research! It is valuable information. Could you please add some pictures here?

 

[w2x3f5]

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

G.Pattonleft 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