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]

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

 

[Kiteretsu_D]

Should i replace benzene with dcm and try again?

 

[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 couldn't find 2b4mp local dealer in my country, thats why i made it, but i think it is right because reaction did happened because when i obtained the powder it was making me cry and my hand was itching, 2nd i used benzene because that what mentioned in the synthesis, i didn't know dcm is much more better option, 3rd yes when i added methylamine temprature was raising i used to add drop when temperature was around 35-40 after adding methylamine it used to go 50-55° then I waited to temperature to come down

 

[freedum]

55 is way too hot. If your base temperature is 25, slowly add while stirring slowly, you keep it hovering around 35. When the full 100ml is added and you're sure the temp isn't still climbing, you can apply heat of 37-38 for 2 hours. You also don't want to overcook, as that leads to a dirtier product. I find I get a very good yield when I follow these.

 

[freedum]

Clean precipitate, almost white.

 

[freedum]

I get a very thin red top, which I could easily vaccum off and would need minimal washing in acetone after

 

[freedum]

This is a comparison of two batches that were frozen for 24 hours. The red top batch was cooked at a higher temperature and for a longer period of time, with not much mind paid to the addition of DCM and heat. The exact timing of the addition of methylamine also was not carefully monitored.

 

[$!$]

Maximum heat dcm is 40°c no more on 2h

 

[Kiteretsu_D]

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

 

[freedum]

Clean precipitate high quality 4mmc

 

[Kiteretsu_D]

Man wish i could make it

 

[Dr. MMX]

1st of all you should just do 2b4m from 4 MP just by leaving that in a solvent for a 4mmc synthesis. I mean it would be easier.
If you wanna do this way you did, you should crystalize it in some solvent to get rid of impurities. You need clean bk4
probably it was very impure and didnt want to react, thats why you got that green color, but its really hard to tell
for sure you cant add warm water, always add cold water when getting rid of methylamine, its more effective.
next time use ice cold acetone before acidification and stirr a mixture

but i believe its all becasue your 4bk didnt react, are you sure it was 50 grams? or it was 50 grams like wet in the photos? then you probably had like 10g:70ml ratio in your flask.
You cant get 4mmc from there, you need to do successful reaction BK4 + MMA to get your mephedrone later you didnt do that so give it another try!
focus to get clean bk4, it should looks like snow crystals if you wanna crystalize it, but you dont need to, you can leave it in solvent that you will use in 4mmc synthesis.

 

[Kiteretsu_D]

50 gram with wetness, i don't know why it didn't get dryed i leave it in air for more than 6 hours

 

[Dr. MMX]

You had to do some mistakes, just try again and read carefully posts that expert shared, you will find the problem for sure

 

[Dr. MMX]

are you sure that you followed the time frames for requried steps? like beeing careful to not add peroxide before before bromide is stirred well enough. Temperature wasnt too high?
did you check what ph you had after using sodium bicarbonate?

 

[Kiteretsu_D]

Temperature was high, when i added peroxide and methylamine, in both of the steps, what is the required temperature?

 

[Kiteretsu_D]

After adding soudim bicarbonate ph didn't changed i guess but after that i added more hcl and then after mixing it reached ph 5

 

[Dr. MMX]

its 55-60 celcius max. Temperature goes high if very large amount of methylamine is added and there is not a lot of solvent, usually its not a problem unless there is DCM synthesis becasue it has to be kept below 36-38. You should have cold water prepared to cool down if you will have temperature problems.
But for such scale I think it was hard to get over that temp, however its always better to measure if you are not sure


What did you do exactly when you were washing crystal for 4bk synthesis? please tell me ur exact steps

 

[Dr. MMX]

There is 1st problem to fix with 4bk synthesis for sure, becasue its reason it didnt react in futher 4mmc synthesis.

Based on photo I think you could have some problems on filtering that via cloth, or using buchner funnel. If you use buchner funnel be sure thats capacity is good for amount of reagent you wanna filter
I think you didnt finish job with your 4bk but you already went for synthesis of 4mmc. Focus on fullfilling each step of synthesis your doing and filter it more slowly, until you receive white crystals. You can check how 4bk should look like on vendors' reagent listings.
Clean 4bk is mandatory to make success in 4mmc synthesis

 

[$!$]

2bromo4m made glass crystal

 

[Dr. MMX]

its problem with 2b4m itself here, it didnt even react, perhaps in EA it would

 

[Kiteretsu_D]

What you mean by i can leave it in bk4? Can you tell me the process or share the link?

 

[Dr. MMX]

You can get 2b4m by adding Br2 to 4MP in a solvent that you will use later for 4mmc synthesis

 

[Kiteretsu_D]

I don't have br2, I'm following different synthesis