A minha síntese de 3-CMC

[mithyl2]

Isto é ótimo.

Porque é que acha que o congelador lhe deu resultados estranhos durante a cristalização?

como é que acha que este método é escalável?

 

[Jesse_Pinkman_]

Por causa da água, quando está a congelar, de onde devem vir os cristais?
O frigorífico normal talvez funcione, mas eu tenho a minha comida lá dentro e não quero limpá-la sempre.
Tentei muitas maneiras de chegar ao produto final e também desperdicei muitos solventes e 2b3c, mas a maneira que descrevi funcionou melhor do que as outras tentativas.
Quase fiquei confuso com todos os métodos diferentes, todas aquelas tigelinhas com misturas diferentes estavam por todo o lado, e eu estava sempre a ver qual é que se desenvolvia bem e qual não.
Por exemplo, quando se coloca ipa gelada na água/pó de cristalização, obtêm-se instantaneamente alguns cristais brancos, mas não são claros e só um bocadinho, por isso tem de se cristalizar novamente e o resto tem de evaporar, vejam a última imagem.
As outras 3 fotos mostram o que acontece com o rm no meu congelador, torna-se 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.

 

[xoxoxoxo]

obtenho cristais de 72g na forma 2b3ch
e 76g de cristais da forma 2b4m.
é muito fácil de fazer para mim.
o mesmo 4mmc é melhor do que 3cmc
em 4mmc é normal dormir e comer, mas em 3cmc é um problema xD

 

[siko]

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

 

[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

 

[SunDay]

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]

What does keto mean? and rm in a recipe ?

 

[Torreto]

How long You wait for evaporate before recrystalization?

 

[SunDay]

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

 

[keras]

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

 

[Jesse_Pinkman_]

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