4MMC Synthesis help

[Tamishea]

Hello dear users

i need done help with my synthesis

I have

2b4m
Ethyl acetate
MA 40% aq solution
HCl 38%
acetone
Dh2o


First i dissolve 100g 2b4m without grinding in 300ml EA stirring 20min until dissolves and heating to 40c, then i pour 200 ml MA 40 with stirring without heating.

my reaction time takes too long about 3/4 hours until i heat to about 50-60c it changes colours. First yellow, dark yellow, green very long , then yellow dark, red, Brown. When i see dark Brown then i pour 450ml dh2o and stir about one minute, then i leave this for about 10/15 min for separate, but they layer is too small equal to the poured ea and 2b4m, the bottom layer is utilized and then ist very dark oil on top. Have i everything done correctly and Please tell me why it takes so long and when possible give me the best way to achieve 4mmc in powder very fast without carcinogen nucleophiles.

 

[loadingST]

With ethyl acetate, you need to distill it off, and treat your freebase to obtain the product.

 

[Tamishea]

But its Not Necessary to Distill off ea. When reaction ist done. Dark Brown Color, i pour dh2o equal to rm volume, and Then everything pour to separatory funnel, wait 10/15 min to separate Layers, bottom Layer will be destroyed and top oil Layer I put in to freezer for about an hour. Then i pour ice cold acetone 1:1 and then hcl acid dropwise in to ph 5,5-6. What im doing wrong at begin that it takes so long. Should i change EA into Something different? I Seen video and reaction is more Clearly but on Video is Used 2i4m, im using 2b4m and it takes really Long

 

[loadingST]

Reflux it and it will be faster, i dont like the precipitation method with ethyl acetate cuz a little acetic acid is formed amd this makes later the product impossible to form nice crystals

 

[Tamishea]

Can you give me one nice recipe from you without ea step by step

 

[Tamishea]

I have overhead Stirrer and magnetisch also, Reflux condenser After ADDING MA 40%?

 

[Dr. MMX]

For such scale no need to. But the vessel should be closed and at least empty of 50%.

 

[Dr. MMX]

You should consider more amount of the solvent. 400-500 ml per 100g of 2 bromo 4 methylopropiophenone, 1st heat it to 30c, then dissolve it. When its fully dissolved there happens short exotermic reaction with sitrring without flushing it on the walls. 30 mins reaction for this should be fine, time of the reaction depends on the stirring and the temperature.

Mixture then is washed in solution 5% nahco3 h2o, then repeated 2-3x for h2o. Aquenous layer is out taken to the waste, organic is to be working witth for futher acidification.

Acetone ice cold 1:1 is poured in while stirring.

For the one mole you use one mole of acid, meaning about 48.5g of 33% hcl aq for 100g of 2b4m, for the safety and precise you should measure ph which remember, will drop very fast from 7-8 to desired 5-6. Acid is added drip by drip.

After you master the reaction and receive good product, you should think to gain a way to do vacuum distilation before its acidified becasue EA reacts with water and hcl which we dont want.

 

[WalterFan]

Don’t heat it next time, do it around 20-30 celsius