Question Failed 4mmc synthesis, need help

[Kiteretsu_D]

Please give it a read and help me

First i did 4mp -> 2b4mp

Chemical i used

4-methylpropiophenone
Hydrogen bromide 46-48%
Hydrogen peroxide 37%
Sodium bicarbonate

(I followed this synthesis - https://bbgate.com/threads/preparation-of-2b4mp-precursor-for-mephedrone.7042/ )

How i did it -
First i added 50ml 4mp to flask jar then added 40ml hydrobromic acid 48%, mix it, then slowly added 18 ml hydrogen peroxide 37% drop by drop while mixing the solution
Then i added cold water
And then filter the crystal
Then washed the crystal with soudim bicarbonate water and then dried the crystal

This is how it looked

Then i did 2b4mp -> 4mmc

This synthesis i followed - (https://bbgate.com/threads/the-simplest-recipe-for-crystal-mephedrone.7031/)

Chemical used -
2b4mp* - 50gg
Benzene - 100ml
Methylamine 40% - 70ml
Hydrochloric acid - 20ml
Chilled dry Acetone -

How i did it -
Added 100 ml benzene in flask then added 50g 2b4mp in the flask, mix it till it dissolved, then added slowly 70ml methylamine 40% to flask closed the lid of the flask and stirrir it using megnetic stirrer for 2 hour then after that i felt asleep after 6 hour again i stirrer it for 2 hour, then after that i stirrer it for 2 more hour, the mixture turned green by now, after that i gave mix it for on and off like every 2 hour i mix for 30 min till i completed 20 hour, mixture was still green

(I didn't use the heating method)

Then i pour the solution into the separating funnel and added 500 ml warm water and mix it then waited for separation then poured out the bottom layer, then repeat this process again
(It is mentioned in the synthesis that i should have a yellow colour solution but I had a greenish-bluish solution, why is that?)

Then i proceeded to the acidification step




I added free base 4mmc solution in the flask and then added chilled dry 200ml dry Acetone, mix it, then added hcl drop by drop to the solution, when i started the ph level was 9, but when i started adding acid its look like ph level was increasing (not sure check pick) after some time its look like ph level reached 3-4, so i didn't knew what to do so i reaserched and and i found out we can increase ph level of by adding soudim bicarbonate water solution to the mixture so i added around 30ml of this solution in mixture, it didn't work so i added more hcl drop by drop i added around 20ml of hcl and after that it somehow reached ph 5-6 i stopped the acidification and mix it for 10 more minutes

(The solution was still liquid it just changed colour green to red, when i added hcl, solution didn't become thick or something like that)

Then i pour out the solution and pack it in glassware and wrap it with plastic and put it in freezer, after 6 hour i took out the mixture and filter it thru paper filter, and nothing happened not a single drop of 4mmc powder was there

It feels so disheartening, after all this waiting and hard work, it didn't work, what do you guys think, what went wrong

I think maybe there could be 4 reason

1. After adding methylamine i should have heated it instead of waiting for 20 hour
2. I should have make the mixture of dry Acton and hcl and then added in the free base instead of mixing freebase with dry Acton then adding hcl
3. I shouldn't have added soudim bicarbonate water solution in acidification step
4. Maybe solution is too much, i should evaporate half of it and try again?

Please tell me what can i improve and what went wrong, and should i throw away the solution or can i still get 4mmc from that solution?

 

[$!$]

your reaction did not react with methylamine at all, the reason may be benzene itself.
in benzen u need heat 2h 40°

 

[Kiteretsu_D]

Are you sure brother? How would i know if it is reacted kr not? Can you tell me what can i do now?

 

[Ihml]

You can test if it’s reacted by using Simons reagent (or any other reagent that can detect secondary amines). If it changes colour to blue, then secondary amine (4MMC) is present.

 

[Kiteretsu_D]

There was no mention of heat in the synthesis, there was said we can wait 24 hour and stir occasionally and it will react? There was no mention of what kind of reaction i should be looking for

 

[$!$]

u cant fix IT. Benzen toulen dcm need heat no wait 24h haha samebody sat u bulshit

 

[Kiteretsu_D]

So i should try again brother? Can you help me with the step did I've done everything else correct tho?

 

[$!$]

Much way is much other steps is to much small steps where u can made mistake. I dont heat any thing only shake 30min and i get freebase wash freebase use acid and także out all solvate out and get puree power this all crystal i made the same day about 2h

 

[Kiteretsu_D]

Can you help me with the step like how do you do it and all, in 2h you made it??? Damn! Would love your help, I'm new to all this have very very basic knowledge of chemistry so many terms I don't understand, but I'm willing to learn

 

[freedum]

It's called a cold synthesis. It's documented here somewhere. But heat is preferable.

 

[freedum]

U don't see much. The colour changes to a more gold.

 

[freedum]

And also that was with dcm.

 

[Kiteretsu_D]

Should i replace benzene with dcm and try again?

 

[Kiteretsu_D]

One more important thing temprature in my city is around 30-35 degrees, when i was synthesing

 

[$!$]

If u mnie how can fix it. Like me.
U need knows what u do in synthesis

 

[Kiteretsu_D]

Damnn looks like someone is in the game for long time, I'm impressed brother

 

[Kiteretsu_D]

Why is it one time green and one time yellow?

 

[freedum]

To begin, the majority of individuals utilize DCM.

Secondly, I am curious as to why you are producing your own BK-4. For your initial attempt, you should eliminate this additional step and simply utilize pre-made BK-4.

Furthermore, your ratios appear to be incorrect. Methylamine should be approximately 100 mL for 50 g of BK-4 (assuming it is indeed BK-4).

The subsequent issue pertains to your proportions for acidification once more. 200 mL of acetone is excessive. Additionally, you are employing an insufficient amount of HCl. The ratio of HCl to acetone should be 10 to 1.

And now, you should combine these components rite before and slowly add them while waiting for the pH level to stabilize between each addition. It appears to me that there was no reaction when the methylamine was added. Is it possible that this is due to the fact that you did not actually make bk4?

From where did you obtain your methylamine? Did you observe an exothermic reaction? Did the temperature rise as you added the methylamine? Did you get a strong smell of methylamine?

Usually, all of these are signs of a reaction. The smell also dies down after mixing for 2 hours at a little under 40ºC.

 

[Kiteretsu_D]

I was wearing the mask so i didn't smell much, it was not that' bad i thought but it was bad

 

[TheVacuumGuy]

Are you sure about that, or is the recipe wrong?

 

[freedum]

Different ph lvl

 

[freedum]

From white clear to this

 

[freedum]

Clean precipitate high quality 4mmc

 

[Kiteretsu_D]

Man wish i could make it