My 3-CMC synthesis

Jesse_Pinkman_

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My 3-CMC synthesis:
at first i want to thank William Dampier for his advices.

I use a sealed glass with a thick toppits foil between lid and glass to prevent fumes.
And no, it will NOT explode, if you use this kind of glass.
I tried with dcm and ethylacetate and both works fine.
The benefit of ethylacetate is the short cooking time, about 20 min.
You do not have to heat it till above 35 degress like with dcm.
But the layers are opposite, water down in ethylacetate and dcm up.
For example:
100g 2b3c
300 dcm
200 methylamin40% aqua
3 hours at aprox 36 degrees
20 min with ethylacetate
After that, open the glass and put same amount as rm, icecold,dest.water /10% sodium bicarbonate inside, this is the first wash to get rid of methylamine.
2 additional washing with dest.water
(same amount as rm)
extract both 2 last washings(water layer) with dcm to get rest of freebase,
then put into rm.
After that, add same amount fresh, cold dest.water into rm, let it stir some time.
Then separate organic and water layer.
I tried different kind of acidificaction.
organic layer alone and organic/water layer together.
I prefer the second one.
Organic layer will be disposed in this case.

put on magnetic stirrer
for acidificaction i use dripping or separatory funnel, drop by drop
(every 2-3 seconds)
till ph6, about 40ml 37% HCI
(i do not mix it with acetone)
While acidificaction the rm begins to change its color from yellow to orange.
After that, separate the water layer with a separatory funnel, put it into a bowl or dish, let it crystallize, this will take some time, 2-3 days.
Freezer gave me strange results so i do not recomend it.
After the crystals have formed, i had different results, sometimes very clear, sometimes light yellow.
So, to get them clear as possible, you have to crush them to powder, wash with acetone, filter with buchner.
Put the acetone into a bowl and let it evaporate, there will be some rest of powder mostly, that will be crushed and washed again.
The washed powder from buchner will be dried and we recrystallize it again.
300ml beaker, 1ml dest.water per 1g powder heated on magnetic stirrer till 60/70 degrees.
Then put Powder into the beaker, let it dissolve and stir 1-2 min.
Then put 2ml ipa or acetone per 1g powder into the beaker, let it stir a short time.
After that, put again into a bowl or dish, evaporate and crystals will form.
Repeat this step until you got the clearness which you want to have.

About the yield (aprox 30-40%, at first i only had about 20%, because i did not re-use the solution after crystalisation), to be honest, i expected more, but maybe my synthesis has some issues or something happened i do not know.
If someone has better experiences, please share your knowledge.
As far as i see here in the forum, many people have questions about 3-cmc but good and helpful answers are hard to find.

The pictures are from different batches and different stages.
 

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mithyl2

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this is great.

why do you think the freezer gave you strange results during the crystallization?

how well do you think this method scales up?
 

Jesse_Pinkman_

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Because of the water, when its freezing, where should the crystals come from?
Normal Refrigerator maybe works but i have my food inside and dont want to clean it everytime.
I really tried very much ways to get to the final product and also wasted a lot of solvents and 2b3c too, but the way i described worked for me better than the other tryouts.
I almost became confused from all different methods, all that different little bowls with different mixtures were standing all around, i always watched, which one develops good and which not.
For example, when you put icecold ipa to the crystalization water/powder, you get some white crystals instantly but they are not clear and just a little bit, sp you have to crystallize again and the rest has to evaporate, look last picture.
The 3 other pictures show what happens to the rm in my freezer, it becomes a solid mass which melts at room temperature, but no crystals.
 

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HerrHaber

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There's also a method for 4MMC recrystallization which employs also NaCl (table salt) in most probably a larger amount of water along the product powder and IPA with also different ratios that you must check. Salty water has a much lower freezing point therefore letting the other component crystalize first since sodium salt is perhaps more water attached but the temperature must NOT reach -18*C or any lower at all costs since salt will also start crystalizing and the more it stays the more salt in the stuff. Hope it helped, I may seek it out for you if you don't find it, cheers!
 

breathing.fire

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Yield You have 30-40 % clean crystals?
 

Jesse_Pinkman_

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When everything works without issues, yes...
 

antrax

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Too low yield, Maybe the pH was not 6, the methylamination was not carried out correctly, you lost product in the filtration, the precursor was not pure enough, or the reagents were not of good quality, there are many hypotheses.
Thank you!!
 

Jesse_Pinkman_

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Yes, i am not a professionell, it was my first time i worked with cathinones and i am sure, results could be better, but i figured out the way, it worked for me. It is just a hobby and i do not try to get a wealthy man from it and to be honest, this work got me bored after so many attempts, but i wanted to share my experience with the community because i saw no similar description for 3-cmc at all.
 

breathing.fire

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Can You share Your method if is yield like this?We are curious
 

xoxoxoxo

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i get 72g crystals form 2b3ch
and 76g crystal form 2b4m.
is real easy to do form me.
the same 4mmc is better like 3cmc
on 4mmc im normal sleep and eat but on 3cmc is a problem xD
 

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breathing.fire

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I don't know maybe my english is not good but I ask how You do this Your method with two solvents and You have yield like this because probably is like with Yeti.Everybody hear nobody see
 

xoxoxoxo

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is the same amost like on 4mmc with benzen and nmp
 

antrax

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To measure pH do you use pH measuring strips or a digital pH measuring device?
For filtration, do you do it by gravity or by vacuum?
To separate two liquids of different density, do you use a separatory funnel?
During the methylamination process, did you close the container so that the fumes do not escape or did you leave it open?
To obtain transparent crystals, did you wash them or what technique did you use?
How many days did it take for the crystals to form and in which container did you leave them to rest and did you close said container or did you leave it open so that the solvent could evaporate?
How much did you pay for the precursor? and the precursor was already ready or you had to buy a pre-precursor and then synthesize the precursor yourself?
Thank you!!
 

UWe9o12jkied91d

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To measure pH do you use pH measuring strips or a digital pH measuring device?
Paper and by smell/color

For filtration, do you do it by gravity or by vacuum?
gravity on muslim cloth/gauze

To separate two liquids of different density, do you use a separatory funnel?
Decant as much water as possible, leaving at least some residues

During the methylamination process, did you close the container so that the fumes do not escape or did you leave it open?
condenser without running water sealed gently with a glove and rubber band

To obtain transparent crystals, did you wash them or what technique did you use?
Precipitation -> Filtration -> Further recrystalization in water + acetone/IPA

How many days did it take for the crystals to form and in which container did you leave them to rest and did you close said container or did you leave it open so that the solvent could evaporate?
Depending on how big and pretty you want you crystals to be you can evaporate a given amount of solvent during re-x, more evaporation and quick cooling = small crystals but smokeable, less evap and gentle cooling = big ones If most solvent is evaporated crystalyzation can take less than an hour, open pyrex container

How much did you pay for the precursor? and the precursor was already ready or you had to buy a pre-precursor and then synthesize the precursor yourself?
No comment
Thank you!!
youre welcome
 

lheartamines

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I wonder what it is about 3-cmc that it seems it's preferable to work in the aqueous layer instead of the organic layer when doing acidification. I also tried your method @Jesse_Pinkman_ and had good results working the aqueous layer. When working the organic layer, I never get salt, just sludge. But I also am working with very small amounts of ketones, around 15 grams. I am trying to perfect my technique as an amateur and do not want to waste large amounts of valuable precursors.
 

ELAIGIBBOR

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Would love to try your synthesis, keep it improving brother
 
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