Ma synthèse du 3-CMC

mithyl2

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C'est génial.

Pourquoi pensez-vous que le congélateur a donné des résultats étranges lors de la cristallisation ?

À quel point pensez-vous que cette méthode peut être mise à l'échelle ?
 

Jesse_Pinkman_

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A cause de l'eau, quand elle gèle, d'où devraient venir les cristaux ?
Le réfrigérateur normal fonctionne peut-être mais j'ai mes aliments à l'intérieur et je ne veux pas le nettoyer à chaque fois.
J'ai vraiment essayé beaucoup de méthodes pour arriver au produit final et j'ai aussi gaspillé beaucoup de solvants et de 2b3c, mais la méthode que j'ai décrite a mieux fonctionné pour moi que les autres essais.
J'ai failli être désorienté par toutes ces méthodes différentes, tous ces petits bols avec des mélanges différents se trouvaient tout autour, j'ai toujours regardé lequel se développait bien et lequel ne se développait pas.
Par exemple, quand on met de l'ipa glacée dans l'eau/poudre de cristallisation, on obtient instantanément des cristaux blancs mais ils ne sont pas clairs et juste un peu, donc il faut cristalliser à nouveau et le reste doit s'évaporer, regardez la dernière photo.
Les 3 autres photos montrent ce qui arrive au rm dans mon congélateur, il devient une masse solide qui fond à température ambiante, mais pas de cristaux.
 

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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.
 

xoxoxoxo

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j'obtiens 72g de cristaux de forme 2b3ch
et 76g de cristaux de forme 2b4m.
C'est très facile à faire pour moi.
le même 4mmc est meilleur que 3cmc
avec 4mmc, je peux dormir et manger normalement, mais avec 3cmc, c'est un problème xD
 

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siko

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hello can you explain how you did this?
the whole process please.
 

HardWork

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Est-il possible de fabriquer du 3mmc en poudre ? Tout le monde parle d'acidification avec de l'eau ou de l'acétone, puis d'évaporation dans un plat. Mais il est peut-être possible de faire comme pour le 4mmc. Il suffit de mettre du HcL directement dans le rm lavé et de former de la poudre. Est-ce possible avec 3cmc ? Et comment le faire avec dcm ?
 

SunDay

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Je ne veux pas vous décevoir, mais non... ce que je sais (j'ai lu tous les sujets sur le 3cmc). Juste la voie de l'évaporation
 
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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
 

SunDay

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In first I want to thank all profs for many advices.
And give my little improvement on 3-cmc synthesis for beginers.
Im acidifying in H2O 1:2 keto/H2O, and after acidification I add 1:1 keto/acetone. Evaparotion going 5 times faster. And after recrystalization(1:1 cmc/H2O) i get 60% yeld of big transparent crystals. It takes just 3days in all. Ofcourse i create perfect conditions, 30 celcs and fan to move air(NOT DIRECT TO BEAKERS) if direct then creates film that dont let evaporate solution.
 

saimon99

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What does keto mean? and rm in a recipe ?
 

Torreto

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How long You wait for evaporate before recrystalization?
 

SunDay

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Next time I will try recrystalization in vodka 40%, will write result.
 

keras

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Any difference if I increase evaporation of cmc in water to make crystals apear or leave it naturaly to evaporate?
 

Jesse_Pinkman_

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Some people mean, its better to evaporate without heating, some say its no problem.
I personally tried with evaporating in an oven on 60 degrees but result was not the same. But you can try and look what suits for you
 
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