Mephedrone (4MMC) crystallization

rado

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Hello everyone!

How can I crystallize a ready-made aqueous solution of mef using NaCl if I didn't have flour initially? Let's say, i have a base of mef in dichloromethane and I'm going to acidify it in excess of water 135 ml per 100 mef, while dissolving mef in water - I do not put mef in flour, but immediately in water

At what stage to add NaCl and in what proportions. According to the upper experience, the author indicates 23 grams per 100 grams of mef, but he has 100 grams of mef dissolved in 100 ml of water. And my oxidation occurs at a figure of 135 ml per 100 g of the product.

How long do crystals form in the NaCl salt solution method? What size fractions are obtained? how long should the product be kept in the freezer? Does the exposure time affect the size of the crystal?

Thank you all!​
 

PolandoEmingarnte

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on dcm you can't do it like that, you need to use water in the acidification process and then use, for example, ipa to immediately start the process of crystallization. Naci is not needed at all, it's nonsense. and you can not freeze because the crystal will not come out in the form of glass and crystal powder only
 
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rado

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Thanks for the reply. I use acetone or ethanol. What are the freezing conditions to get large crystals with a 1 to 1 yield? Let's say I got an aqueous layer of mephedrone, diluted it with acetone or alcohol - how then is it better to freeze? If you immediately immerse -18 in the freezer, you will get a fine crystalline powder. How then to get large crystals quickly? Now I get large pure crystals only when this solution evaporates, but this is a long process
 

PolandoEmingarnte

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What kind of crystals do you want to get? you can use the form of needles but do not use a freezer and it lasts 24 hours, but still some of the solution must be evaporated to recover the rest of the product.
 

rado

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Hi bro. Now I get such crystals only by evaporation. But I am not satisfied with the timing if the layer is large. You say you can evaporate 50% and then into the freezer - will the crystal that will fall out from the remainder of the solution be strong or will it just be a small fraction, whereas large crystals already exist after evaporation.

Is there a way to grow crystals of stones if 1 kilo of mef is dissolved in water 1300 \ acetone 200. There is no equipment to evaporate - how to freeze properly right away and will it be convenient?
 

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PolandoEmingarnte

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the biggest mistake is the wrong proportions then and you have to wait for weeks - water evaporates longer and acetone faster
 

rado

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I can't acidify with less water, when oxidized, less water simply won't take all the mef from dichloromethane. Do you have a solution for oxidation to an aqueous layer with different proportions?
 

rado

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Hello everyone, brothers! I will pay for help in obtaining information on the crystallization of mephedrone from the water layer in various ways. Evaporation from water has already been tested - this is a long way, there is no rotary evaporator yet, so we need faster methods without losses
 
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Has anyone tried the emergency freezing method with Dry Ice (CO₂)?
If anyone has a chance, please try it and post the result here.
Method:
The ratio of water/4 mmc is 1 mL /1 g. Dissolve 4 mmc in water and bring to boil. You can add 200 mL of IPA per 1 liter of solution.
Place a 2 L plastic bottle filled with ~500 mL in a dry ice bucket. A crystal will quickly form instead of liquid. To get it out, gently cut the bottle open. The crystal then needs to be dried in dry air.
 

rado

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How can I get crystals of this shape? This is definitely freezing, not evaporation! What are the proportions? How to get it immediately from the water layer, if there was no flour initially? What kind of solvent to add - I am ready to buy all this information if there is a ready result!
 

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leon

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Hi everyone!
If my 4mmc not nice white or glass then i throw cold acetone and leave there 2h ?
Other I have glass nice crystal but i find little brown spots in upper layer. whats the problem?
 

Toribius

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What about disolving 4mmc in methanol and a a small portion of acetone?
 

noMercyy

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Hello, can someone explain me, why the 3cmc cristals whitening over time? (in this case 2-3 days after recrystallization) And is any idea how to prevent it or make it stable/permament without whitening?
 

Metribolone

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I am wondering if after purification and recrystalization, if the product is then melted and allowed to cool, would larger crystals form or would it be more like a pancake that would have to be broken up.
 

WillD

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Perhaps the water was not the best purity. Ethanol sometimes works better so that there is no oxidation. If there were impurities in the powder, after dissolving in water, you can extract impurities with a solvent (toluene or other solvent not mixed with water) and then add alcohol to the water and crystallized.
 
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