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

[dark_side_of_chemistry]

In 2bromo 3 chloropriofenon synthesis is the same ?

 

[RichKuklinski]

it is same

 

[Rocco666]

N

 

[Rocco666]

No

 

[William D.]

yes

 

[whitelabel]

@William D. Is the 4mmc light sensitive? Would it lose potency if dried in the sun?

 

[Serega]

I get the purest product in DCM, but the main thing is not to let the solution boil, keep the temperature no higher than 36C (4-mmc turns out to be impeccably clean and snow-white). Another great option is dichloroethane. also a good result is obtained when using NMP and toluene together (3:2 ratio).

 

[crisu1542]

What about the DMF ? Do I have to keep the temperature to 36 degrees Celsius here too ? As far as I know the boiling point of dmf is over 130 degrees.

 

[malignoalfa]

About the video, someone would know to say:

1) Which mechanical stirrer is used? Top mechanical stirrers often look like a metal rod rather than PTFE.

2) How is the emptying done in the system? through which RBF tubing?
See that the system has negative pressure and he uses this to feed the RBF with reagent liquids through a hose.

Thanks!

 

[G.Patton]

Hi, not so matter. I would recommend you to use PTFE if it possible.
Use vacuum pump and silicone hose. What is problem and what don't you understand?

 

[QAZ123123]

A hose should be connected to the top of the reflux condenser, and the hose should be connected to the vacuum pump.This is where the vacuum comes from.

 

[wikimiki]

What if I gonna replace NMP with DMF? Somebody tried? What proportion of DMF should be used if in use instead DMF?

Somebody have the stirring timings and than other timings for those synthesis description? It looks very interesting, I will be appreciate.

 

[William D.]

DMF can be used like DMSO, but yield and some other conditions may differ.

 

[lemon]

DMSO+Toluene = Yield

 

[wikimiki]

William thanks a lot but could you tell me how much differ your recipe if I put DCM and what need to be changed if I put as someone said below DMSO and Toulene? I will be appreciate. With highest respect for the recepture you have posted I cannot get how in large scale production the 40-50% of yield can satisfy you?

Best regards

 

[William D.]

For the test, you must mix BK4, dcm and methylamine as usual. You can add the amount of DMSO until the mixture becomes homogeneous. In this form, the reaction will be faster than usual. You control the reaction for the first time in temperature (when the mixture begins to cool, the reaction is finished, even without additional heating). After you add pure cold water and separate the lower layer and rinse again. Further steps are the same as you used (acidification with acetone or into the water layer)

 

[crisu1542]

1. when swapping NMP for DMF, are the temperatures and pH different ? Solvents have different boiling points and I don't know if this is relevant.
2.Finally, what should be the temperature after adding methylamine ? Once it finds 36, once it finds 40.... Need exact information.
3. is it necessary to heat externally or to cool the solution after adding methylamine ?
4. when acidifying use EA or not ? Once I read that no, once that EA instead of acetone.
5. does the free base if it does not exceed 36 degrees Celsius does not require further cleaning ?

Thanks to all experienced in advance .

 

[NieDoswiadczony]

40% roztwór wodny aminy metylowej (CAS 74-89-5can you replace it with something?

 

[As88]

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 - What are you using to heat the mixture to 40 degrees at the above point?

 

[G.Patton]

Temperature control jacket for the batch chemical reactor.
hi

 

[QAZ123123]

Mephedrone synthesis (4-MMC) in NMP solvent. Large scale. The method and materials​

Mephedrone hydrobromide synthesis no the same​