Meine 3-CMC-Synthese

[mithyl2]

Das ist großartig.

Warum glaubst du, dass der Gefrierschrank bei der Kristallisation seltsame Ergebnisse liefert?

Wie gut lässt sich diese Methode Ihrer Meinung nach skalieren?

 

[Jesse_Pinkman_]

Wenn das Wasser gefriert, woher sollen dann die Kristalle kommen?
Ein normaler Kühlschrank funktioniert vielleicht, aber ich habe meine Lebensmittel drin und möchte ihn nicht jedes Mal reinigen.
Ich habe wirklich sehr viele Wege ausprobiert, um zum Endprodukt zu kommen und habe auch eine Menge Lösungsmittel und 2b3c verschwendet, aber der Weg, den ich beschrieben habe, hat für mich besser funktioniert als die anderen Versuche.
Ich wurde fast verwirrt von all den verschiedenen Methoden, überall standen verschiedene Schälchen mit verschiedenen Mischungen herum, ich habe immer geschaut, welche gut entsteht und welche nicht.
Wenn man z.B. eiskaltes Ipa in das Kristallisationswasser/Pulver gibt, bekommt man sofort weiße Kristalle, die aber nicht klar sind und nur ein bisschen, sp muss man wieder kristallisieren und der Rest muss verdampfen, siehe letztes Bild.
Die 3 anderen Bilder zeigen, was mit dem rm in meinem Gefrierschrank passiert, es wird eine feste Masse, die bei Raumtemperatur schmilzt, aber keine Kristalle.

 

[HerrHaber]

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!

 

[NeoTolls]

How much NaCI u use ?

 

[lheartamines]

Seien Sie vorsichtig, wenn Sie ein digitales ph-Gerät und DCM verwenden, denn wenn Sie es während der Überwachung in der Kammer lassen, schmilzt es das Gerät.

 

[Jesse_Pinkman_]

Ja, ich hatte das mit einem Thermometer

 

[TheVacuumGuy]

I've had this too. Solved by getting an expensive glass probe

 

[misteroil]

Hello guys, maybe someone could help me with situation..?
Ratio of chemicals 1:2br3cl, 3: DCM, 2:MA. stiring for 3hours in 37c. All the time reaction went well, in the end yellow/amber collor of base.
But this time i have very low temp in lab, and i pour all MA in 15mins. All substance temp raised just too 27 degree. Then I put rm to warm bath and raised temp to 35. After 2 hours stiring all was going well. But in next hour all rm turned PURPLE. Acidifying in dem.watter and get purple watter layer. Now i see that my crystals will be purple. How could i wash it? becouse i think that there was much not reacted chems, but wich, i dont know.

 

[JosephBratan]

Hey $!$

 

[TheVacuumGuy]

Hey $!$

 

[pamrz]

Hi Guys,
Im trying 3cmc and I have questions about acidification. I'm working on organic layer - but nothing forms. Made few attempts, some was good most of them not, I cannot realize where is the problem.

1) on which temperature shoud be freebase acidified? Room temperature or is should be cold before acidification?
2) It's better acidifi before or after adding cold acetone ? Is aceton necessary on DCM?
3) I'm on PH 6 and I have very dark liquid, after 12hours in freezer nothing happen (but it must be there, when PH paper dry, there are white crystal layer)
4) Is way add destilled watter to liquid and separe water and let i crystalize?
5) can be separated acidified/ DCM/Acetone/ liquid reuse somehow?
Thank you

 

[Jesse_Pinkman_]

I think, you did not read or understand the process...after acidificaction, you dispose the organic layer, the water layer contains the product and you need to evaporate the water

 

[Jesse_Pinkman_]

Acetone is not necessary, for 4-mmc it is. So, read my recipe, try to understand, what happens there...acidificaction should be at low temperature, dest water from freezer, can also use dest water ice cubes to cool down the rm while acidificaction. Hcl drops every 2-3 seconds 1 drop

 

[pamrz]

Thats the point. I used way that I know from 4mmc.
But product will dispose to water AFTER accidification isnt it?

 

[Jesse_Pinkman_]

Yes, chloro switches to water when ph 6 , organic layer is not necessary then

 

[pamrz]

And about ratio for preparation:
100g 2b3cl / 300ml DCM / 200ml methylamine 3hrs on 38degrees - nice orange colour of bottom layer.

 

[Pinkbay]

Hello friends.
I put it in the refrigerator for 12 hours after acidification and got some salt with different shapes, but when filtering, the salt disappeared and turned into liquid. Does anyone know the reason?

 

[Jesse_Pinkman_]

Read the recipe...no refrigerator, evaporate the water layer

 

[SunDay]

Hello partners..
Im out of stock 2br3cl, but have 2br4m... On mephedrone I was working with toluen in the old days, droping flour..etc..
Now I will work with DCM and watter layer, now reading what best for meph. So in couple post above Jesse mentioned that in mephedrone we need acetone in step by acidification. I want to ask why, and when. Thats the evaporation of watter layer would be faster? becouse acetone mixes homologue with watter... Or we dont need watter at all?

 

[dnBQByvHb8Zkawbjpx]

Hello there,
After amination in DCM you discard the water layer, repeatedly flush the organic layer with water to remove excess methylamine and you always keep the 4mmc free base in DCM. Acetone is then added 1/ to dilute the free base in order to provide better thermal stability so it does not heat too fast as HCl is added, and 2/ to wash away DCM and any impurities soluble in acetone from the precipitate. Acetone is used since it does not dissolve 4mmc.HCl and dries fast without leaving residue, and it's cheap.