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

[WillD]

Can acetone be replaced by IPA?

phantomwriterYes, but in small quantities. Otherwise, you will have to evaporate alcohol.

What equipment is used for large scale production?

Large glass reactors, or equipped plastic barrels

 

[Toribius]

Yes, but in small quantities. Otherwise, you will have to evaporate alcohol.

Large glass reactors, or equipped plastic barrels

William DampierCould you please explain this equipped plastic barrel thing?

 

[csigger]

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

 

[DrugZ]

Guys, from where you get these reagents?

 

[HerrHaber]

Guys, from where you get these reagents?

DrugZChemicals 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.

 

[Sailor]

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?

 

[UWe9o12jkied91d]

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?

SailorYes, bicarbonate wash also adviseable once

 

[Sailor]

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]

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

 

[jarodleto]

peut-on changer le benzène en toluène ? si oui combien s'il vous plait

 

[mocnykutas]

peut-on changer le benzène en toluène ? si oui combien s'il vous plait

jarodletoEnglish

 

[jarodleto]

English

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

 

[UWe9o12jkied91d]

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

jarodletoIf 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]

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.

UWe9o12jkied91dChouette, ca me fait rigolle... mais il fait avoir reson.

 

[mocnykutas]

When u throw to much acid u get it.
Need wash good and later i show what we get

 

[mocnykutas]

600g guy WHO i teach made

 

[HerrHaber]

600g guy WHO i teach made

mocnykutasI wish for teachlings like this, hit me up if anyone interested in lessons.

 

[crisu1542]

I wish for teachlings like this, hit me up if anyone interested in lesso

HerrHaber

 

[ice4mmc]

600g guy WHO i teach made

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

 

[freedum]

600g guy WHO i teach made

mocnykutasLooks dirty as hell

 

[JuanoImano4378]

Reaction scheme:

View attachment 1218 ​

Reagents:

• 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) - 5 kg;
• n-Methyl-2-pyrrolidone (NMP; cas 872-50-4) - 20 L;
• Methyl amine 40% aq. solution (cas 74-89-5) - 8 L;
• Benzene - 20 L;
• Acetone - 30 L;
• Hydrochloric acid con. aq. solution (HCl 36%) ~ 1.5 L;
• Distilled water - 20 L;
• Magnesium sulphate (MgSO4);

Equipment and glassware:

• 100 L Batch reactor, which is equipped with drip funnel, top stirrer, thermometer, temperature control system (cooling) and reflux condenser;
• Funnel;
• pH indicator papers;
• Several buckets 25 L;
• Barrel 100 L;
• Beaker 2000 mL;
• Vacuum source;
• Scale;
• Measuring cylinder 1000 mL;
• Glass rod and spatula;
• Scoops;
• Nutsche filter;
• Rotary evaporator;

Download Video

Mephedrone hydrobromide synthesis

• Novator
• Aug 17, 2022
• 22
• 2-bromo-4'-methylpropiophenone 4-mmc bromoketone cas 1451-82-7 meph mephedrone mephedrone hydrobromide mephedrone hydrochloride n-methylpyrrolidone nmp

Mephedrone hydrobromide synthesis from 2-bromo-4'-methylpropiophenone with n-methylpyrrolidone...

​

Synthesis procedures
1. 2-Bromo-4'-methylpropiophenone 5 kg is poured into Batch reactor or another crude 2-Bromo-4'-methylpropiophenone amount after halogenation reactions.
2. n-Methyl-2-pyrrolidone 20 L is poured into the reactor. Top stirrer is turned on and the reaction mixture is heated up to 40 °С.
3. When temperature is reached 40 °С, methylamine 40% aq. solution 8 L is poured into the reaction mixture and stirred for 20 min.
4. Next, distilled cold water 20 L is poured into reaction mixture and stirred for few minutes.
5. Benzene 15-20 L or other suitable solvent is poured into the reactor, the mixture is stirred for few minutes.
6. Than, the stirrer is stopped, the mixture is divided into two layers.
7. The bottom aqueous layer is drained through the bottom valve of the reactor. Top layer is drained into a bucket and dried over MgSO4. Than, dry solution is poured in another bucket.
8. Ice acetone 20 L is added to the reaction mixture and hydrochloric acid (HCl 36%) is added dropwise with a constant stirring to reach pH 5.5-6.
9. The mixture is put into a freezer for 12 h.
10. Crystallized mephedrone hydrochloride is filtered on a Nutsche filter and air dried. The yield is 58%.

Note
NMP can be replaced by DMSO, DMF, Sulfolane.

William Dampier
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]

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]

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?

 

[eddycordon]

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?

Charlie3This is Want i get 4mmc crystal