Minha síntese de 3-CMC

[mithyl2]

isso é ótimo.

Por que você acha que o freezer deu resultados estranhos durante a cristalização?

Como você acha que esse método pode ser escalonado?

 

[Jesse_Pinkman_]

Por causa da água, quando ela está congelando, de onde devem vir os cristais?
A geladeira normal talvez funcione, mas tenho meus alimentos dentro dela e não quero limpá-la toda vez.
Realmente tentei muitas maneiras de chegar ao produto final e também desperdicei muitos solventes e 2b3c, mas a maneira que descrevi funcionou melhor para mim do que as outras tentativas.
Quase fiquei confuso com todos os métodos diferentes, todas aquelas tigelinhas diferentes com misturas diferentes estavam espalhadas por toda parte, e eu sempre observava qual delas se desenvolvia bem e qual não.
Por exemplo, quando você coloca ipa gelada na água/pó de cristalização, você obtém alguns cristais brancos instantaneamente, mas eles não são claros e apenas um pouco, então você tem que cristalizar novamente e o resto tem que evaporar, veja a última foto.
As outras 3 fotos mostram o que acontece com o rm no meu freezer, ele se torna uma massa sólida que derrete à temperatura ambiente, mas sem cristais.

 

[HerrHaber]

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

 

[HardWork]

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]

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

 

[SunDay]

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]

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]

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.

 

[HardWork]

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

 

[Jesse_Pinkman_]

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]

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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