Synthese van mefedrone (4-MMC) uit haloketon in ethylacetaat. 1-10 kg Schaal.

[yin-yang]

N-methylacetamide zou oplosbaar moeten zijn in aceton, maar ik kon niet vinden hoeveel. Freebase is inderdaad zwart en het resulterende poeder wordt groen bij toevoeging van een kristalliserend oplosmiddelenmengsel (niet gereageerd keton?). Het is veilig om aan te nemen dat dit niet de schoonste procedure is.

Sommigen zweren dat elke andere reactie dan die waarbij NMP als oplosmiddel wordt gebruikt, veel, veel slechtere resultaten oplevert in het eindproduct. Meer een snelle high zonder euforie.

Heb je GC-MS gedaan om te zien of er onzuiverheden in het resulterende poeder/kristallen zitten?
@G.Patton
@Marvin "Popcorn" Sutton
@William Dampier

 

[Wan Jack]

(6.The stirring is stopped. The reaction mixture is left for layer separations. A bottom layer is drained through a bottom reactor tap..)Because of the excess methylamine, the free base was washed more than 3 times with more than 2 times the deionized water.

 

[StarWars]

8. Daarna wordt het mengsel verwarmd tot 55 °C.
in de video staat duidelijk dat het niet nodig is om op te warmen. en hier schreef iemand om het dan op te warmen voor wat als het mengsel zelf de temperatuur bereikt niet hoger dan 65 °.

 

[G.Patton]

Hallo, 55 graden *C is nodig om vacuüm verdamping van oplosmiddelen en methylamine overschot. Het is een optionele procedure.

 

[goku1008]

can i skip this i dont have vacuum systume
and plz give me your screenshot video link plz

 

[G.Patton]

This video in the topic, dude...
Yes, you can separate layers without vacuum. There is this information in the screenshot.

 

[goku1008]

Stage 2
4. The stirring is stopped. The reaction mixture is left for layer separations. A bottom layer is drained through a bottom reactor tap.

I'm asking ethyl acetate is light solvent and 2b4m is heavy so why we need to drain bottom layer
If we drain bottom layer then only ethyl acetate left in flask
Help me on this plz plz

 

[goku1008]

stage 2
3. The mixture is stirred until complete amount of 2-bromo-4'-methylpropiophenone (cas 1451-82-7) is dissolved.
4. The stirring is stopped. The reaction mixture is left for layer separations. A bottom layer is drained through a bottom reactor tap.


my qustion is in video bro do this step after mixing water .but in method layer happen after 2-bromo-4'-methylpropiophenone dislove in ethyal cant understand this point

 

[G.Patton]

Hello, I edited the write up. You should separate layers at step 7.

 

[William D.]

When you received BK4, you must separate water with acid, which remained in the reaction mixture. To do this, we dissolve the BK4 and separate the residue of water.

 

[goku1008]

in vidoe after addingmethylamine 40% Colour change green red brown happened. Im asking is that same happen with 2b4m
also in video stating they said bk/ik .
is bk means 2b4m and ik mens 2i4m

 

[Naruto]

No

 

[goku1008]

then explain what is bk/ik ?

 

[Naruto]

Is other precursor and on 2b4m oil is yellow is is green then no all 2b4m work good

 

[G.Patton]

2-Bromo-4'-methylpropiophenone
2-Iodo-4'-methylpropiophenone
These are two different 4-MMC precursors. Please, look through the Methcathinones section topics before ask next question!

 

[William D.]

It is better to use 2br4mp, it is cheaper and gives a greater yield.

 

[dodobird]

Hi everyone

FILTRATION QUESTION

Once I have the slurry mixture out of the freezer after 8 to 10 hours....
What are the easiest alternate ways to wash with acetone and filter quickly assuming I do not have a vacuum pump at hand and need it dried into chunks quickly??

Some options like pressing out the liquid or perhaps some light heat on a hot plate after putting in a pan and using a spatula to stir it constantly?? OR using a muslin cloth to squeeze out excess liquid then placing under a small slow fan with indirect heat source for quicker drying??

This is the only hurdle I foresee in my synth starting next week once I have the 2b4m in hand. Please give me some reasonable options guys.

@William D. @G.Patton @StarWars

 

[Dr. MMX]

You could use the cloth or some kind of the filter, put it into the freezer (so the product isnt dissolved). After some hours it should be filtered.
As you said, you could press it by pushing as well.
Remember if temperature will be more warm - product may dissolve.

vacuum source is prefered, reason is that job is simplier and you will keep more product (usually) as long it will be still ice cold, while filtered.

Addictional accetone is used, when the filtrate is not "clean".

 

[dodobird]

Sorry forgot this info... gonna give it a second go next week just wanted to work out any kinks in my head as I jeep visualising the steps.
You guys cannot fathom how much help u all are. Kudos

 

[dodobird]

HEllor
Hi

Great post very clear, I have some questions though..

Once the precipitate is washed with soda pus water and then with water and filtered, does ot matter if it is not completely dry, can I proceed with ethyl acetate and them amination witin an hour of straining using a cloth for filtering and air dried with a fan

Is it better drying if I put this crude slightly wet bk4 in the fridge or freezer

Please help

 

[dodobird]

My bad kinda forgot yesterday's reading. Mindfog is setting in quickly with age lol

 

[dodobird]

Replied to the wrong post admit..sorry

Was referring to 4mp to 2b4m synthesis before ea and amination.

 

[G.Patton]

It's worth to use dry bk4 in opposite case you'll have mistake in your measurements