Meine 3-CMC-Synthese

mithyl2

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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_

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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.
 

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HerrHaber

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it depends on how much material you want to dissolve and the water to alcohol ratio.
 

HardWork

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Is it possible to make 3mmc in powder ? Everyone is talking about acidification with water or acetone and then straight to dish and evaporate. But maybe it is possible to make it like 4mmc. Just putting HcL straight to washed rm and powder forming. Is it possible with 3cmc ? And how to do it with dcm ?
 

SunDay

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I dont want to disapoint you, but no... how much i know ( i read all topics about 3cmc). Just evaporation way
 
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SunDay

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But its strange, becouse everythime when i wash stuff with acetone I put acetone to fridge, and after some time i get 3cmc powder. why its not happening when acidifying with acetone from begining..?
 

HardWork

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I have tried reaction with toluen,and then tried to put only HCL,so I’ve got some powder. But yield was only 25%
 

SunDay

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I tried this also. 1st time my HCL was 80% (it perfectly fits for H2O acidification in proper amount) but when only HCL, everything BURNT :)), and second time with 26-38% so drop was sticky flufy mass(then you need MUCH work to get crystals from this shit, and yeld was about 35%.
By the way, in market there is 28% HCL, it comes from latvia.. that shity HCL makes problem with acidification, purple or emerald color goes on, and really hard to achieve optimal ph. All latvian chem in shops ar shit, so dont be fooled.
 
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HardWork

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Yeah,I have used 26-38% hcl and get 25% yeld.
 

Jesse_Pinkman_

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Same, always had 25-30% after several washing and recrys...there are methods with more yield for sure, but my experiences were always around this amount
 

EL Mayo

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Then u how made u get only 30% haha I get minimum 60% i wait week and get crystal if i need powder easy get out in freezer form dark Orange oil all water take out
 

EL Mayo

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.
 

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