Mephedrone synthesis (4-MMC) in NMP solvent. Large scale.
benzene is carcinogenic record video of 4mmc production using nmp benzene is fun and inefficient 40% of the final product very little per 100g bk4 you need to use a 2l flask I use a 2l glass bottle and it yields 300g and 350g of the final crystal product. If you are using benzene toulen dcm xylene nmp you must use different cooking temperatures and the time is different. I do not use a flask, but an ordinary wine bottle, a bucket, a conical separator for wine, cloth for filtration and a centrifuge for drying clothes.
Hello everyone. All the synthesis is going well until acidification. Initially everything goes correctly, a "flour" precipitates, but with the addition of HCL 36-38% the whole mixture initially becomes red until it turns strongly blue.
Such soiled gunpowder can not be washed even with a huge amount of acetone, minimally the blue color comes off, but the final product is still strongly blue, and the yield is drastically low.
When souring, will diluting HCL with acetone, for example, in a ratio of 1:5 help? Of course, the whole thing frozen using dry ice.
The second question is, when adding methylamine, should I add it in small portions so that the temperature does not exceed 60 degrees, or can I pour it all at once and not look at the temperature? Adding all the methylamine at once won't drastically reduce the output?
Greetings
Such soiled gunpowder can not be washed even with a huge amount of acetone, minimally the blue color comes off, but the final product is still strongly blue, and the yield is drastically low.
When souring, will diluting HCL with acetone, for example, in a ratio of 1:5 help? Of course, the whole thing frozen using dry ice.
The second question is, when adding methylamine, should I add it in small portions so that the temperature does not exceed 60 degrees, or can I pour it all at once and not look at the temperature? Adding all the methylamine at once won't drastically reduce the output?
Greetings
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In point 8, I add 20L of ice-cold acetone to the reactor and only separately add HCL 36-38% slowly until the pH drops to 5? Do I mix the HCL with 20L of acetone and only add the mixture to the reactor?
I can't figure out why during acidification the whole thing precipitates nicely until at some point it starts turning blue....
I bet it is due to adding too concentrated HCL 36-38% by which I burn the product and hence the blue mess.
I can't figure out why during acidification the whole thing precipitates nicely until at some point it starts turning blue....
I bet it is due to adding too concentrated HCL 36-38% by which I burn the product and hence the blue mess.
- By plancklong
You are dropping the pH to 5. That is too low! The procedure says only drop to 5.5 - 6. Next time, bring the pH to the correct range and see if you have blue then!
Final blue color yes, but the liquid was not all red as in the attached photos. Normally yellow oil, white gunpowder precipitated, over time the yellow oil began to turn blue while staining the gunpowder, which could no longer be cleaned with acetone. Ultimately, after draining, the blue powder looked like this in the last photo
I honestly have no idea, I haven't checked it. In the next few days I will try to approach this synthesis again I will check it and let you know.
In my opinion, it is the fault of acidification with concentrated undiluted HCL by which the product burns and impurities are formed. Now I will want to add ice-cold acetone at step 8, and acidify successively with a 1:5 HCL:Acetone mixture. It seems to me that this will solve the problem.
The organic phase takes on a nice orange-amber color so I would argue that it is running at least correctly.
In my opinion, it is the fault of acidification with concentrated undiluted HCL by which the product burns and impurities are formed. Now I will want to add ice-cold acetone at step 8, and acidify successively with a 1:5 HCL:Acetone mixture. It seems to me that this will solve the problem.
The organic phase takes on a nice orange-amber color so I would argue that it is running at least correctly.
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