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.

 

[CARLITOBRO]

Anyway i have some questions here if you dont mind and thank you in advance

1. Used 20gr of bk4 in 100ml ethyl acetate in 500ml round bottom flask reflux attached in a water bath 40c-60c waited till all bk4 dissolved and temp reached 50c in the water bath added at once 100ml of 40%aq methylamine let it reflux for 45min and added 150ml of water and separate the organic ( by the way it was so poor yield not even 10ml yellow oil).

2.Removed while still a bit hot added 20ml ice cold acetone and begin adding 33% hcl drop by drop the solution becomes RED and quicly turned green

1.WHAT AM I DOING WRONG there is no color change after adding methyl 40%aq with stirring it just goes from opaque to yellow after 30min

2.when using ethyl acetate and methylamine aq 40% is it better to heat up with stirring OR the opposite cool it with water bath and keep to reaction cool ?

3.before acidification and ice cold acetone adding to the organic solution is it better to cool the organic phase after separating in the fridge or just added the ice cold acetone ?

 

[WalterFan]

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

 

[CARLITOBRO]

Thanks and its done....got beaaaaauuuutiful flakes after acidification ...and it gets u hiiigh as fuck

 

[Tamishea]

Hello dear Users. I Think Reaction is done properly, but why ph drop to 1 after acidification then is red and then first milky brown… i dont know but i can confirm that everything Works Fine.

 

[WalterFan]

It’s not fine, when you doing acidification, the temperature would go up, monitor your temperature during acidification

 

[Miś.Didi]

Hi Boys.
I'm do the same way but i put there NMP no to much.This staff have powder!!!

 

[andy.hug]

What method You use to make this stones from photos

 

[Miś.Didi]

I use EA+NMP and methyloamine hcl and naoh+water

 

[dnBQByvHb8Zkawbjpx]

It's about the crystallization technique, not the reaction. I get these "rocks" when I dissolve 4-MMC powder at higher temperature (1:1 by weight in water) and allow to cool down to room temp. These rocks form within few hours but to me they are inferior to slow-grown crystal over days or weeks. These rock form by quickly crashing out a lot of matter out of the solution. It's like millions of tiny needles form rapidly and create this kind of a mesh or sponge structure. It is not very dense and traps a lot of mother liquor inside. They take a long time to dry and soak up acetone during washing. When time allows it I prefer to use double amount of water, dissolve at room temp and allow to crystallize over days or few weeks.

 

[andy.hug]

Yes I ask about crystalization method.Waht mwthid You propose for nice crystals.What proportions powder:solvent,temperature in room and layer in box

 

[dnBQByvHb8Zkawbjpx]

In general the size of crystals is proportional to the time allowed for them to form. There is no shortcut to grow nice large true crystals in a short period of time.

My preferred solvent is just demineralized/distilled water as it's cheap and gives no odor. Use as much water as you need to fully dissolve 4-MMC powder at room temperature, 2:1 ratio by weight (water-powder) is generally enough or perhaps a tiny bit more than required but that's what I use. Stir until the solution is clear and then let in a well ventilated room undisturbed with no heat applied. After some initial water evaporation a sheet of thin crystal will form at the surface of the liquid and then grow stronger. There must be some depth of the solution so it does not dry too fast. Plan at least 5 days, maybe a week or two, if you want some nice crystal. Remove grown crystal and continue with the remaining liquid in a smaller box until it's all used.