Mephedrone synthesis (4-MMC) in NMP solvent. Large scale.

WillD

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Yes, but in small quantities. Otherwise, you will have to evaporate alcohol.
Large glass reactors, or equipped plastic barrels
 

Toribius

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Could you please explain this equipped plastic barrel thing?
 

csigger

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At the end, can I do the acidification by bubbling hcl gas into the free base?
 

DrugZ

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Guys, from where you get these reagents?
 

HerrHaber

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Chemicals are obtained from one another by a fundamental process known as learning chemistry and being good at it. Alternatively you document what you can't make yourself and there are people here with what you want or what is needed to obtain what you want.
 

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Serega posted, that with his DCM approach you only need to rinse the freebase 2-3 times with cold water to remove the methylamine residue.

When exactly needs this to be done? After the aqueous layer is drained, just do 2-3 more plain distilled water washes before drying over MgSO4?
 

Sailor

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When replacing NMP with DCM as well as ethyl acetate instead of acetone, is it still necessary to add benzene before letting the layers divide?
 

mocnykutas

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Bulshit bulshit. Bromoketon with solvate. Mix 1 day. Look like freebase but is not need use methyloamine later
 

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jarodleto

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can benzene be changed into toluene? if so, how much please?
 

mocnykutas

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English
 
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jarodleto

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Sorry, Can i change the benzene with toluène ? If so, how much quantity
 

UWe9o12jkied91d

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If you are not achter le bromoketon and halogenate yourself then yes, toluene is suitable.If you are starting from bromketon you can dissolve directly in nmp/dmso and proceed to add methylaminating agent.Once you think it’s done reacting you add water and toluene/ethylacetate , leading to separation of the mixture in 2 layers.
 

HerrHaber

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That makes me laugh... but it's got resonance.
 

mocnykutas

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600g guy WHO i teach made
 

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ice4mmc

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@mocnykutas can you give me a wickr.me/singal? I have some question i gonna pay for your time. (PL)
 

JuanoImano4378

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Hi, I'm using Ethyl Acetate in place of Benzene here. I noticed in the synthesis that evaporation/distillation of the solvent is not mentioned after extracting top layer (step 7). In the video, it was mentioned that we should. Is it not necessary? What can I expect if I did not distill the solvent, is it just a longer freezing time during crystallization (step 9)?
 

HerrHaber

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Ethyl acetate is a very practical solvent but it's limited by high concentrations of stronger weak bases (MeNH2) or even dilute solutions of strong bases (KOH) same with acids, always work as quick as possible when you have the pH far from 7 thus rotavap before acidification may help when processing a large batch but I would do it quick and evap only half the stuff or so... DCM is way much better for this and also boils under 50C. The solution to be acidified is best dilute with cold acetone or'and ether with the acid also diluted or not depending on quantity, maybe even gasing it may be a better option if you make a lot. Benzene is to be avoided at all costs, toluene and xylene make stuff blue/black. I never trie DCM along with AcOEt in a mixture then quickly evap (from a crystalizing dish with stirring on heat or water bath for safety of the product), the ratio I guess it's crucial since one sinks to the bottom and the other floats above water so it is safer to perform in one of them and then extract the water layer with the other.
 

Charlie3

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Ive tried this synthesis accordingly to the manual, only difference was that i replaced benzene with EA.

100g 2bromo4
400ml NMP
160ml methylamine
1litre water
400ml Ethyl acetate

600ml acetone
HCL added till PH6

the total amount of salt ive got was only about 25g. Not crystals yet.

anyone know what went wrong?
 
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