Mi síntesis de 3-CMC

[mithyl2]

esto es genial.

¿por qué cree que el congelador le dio resultados extraños durante la cristalización?

¿crees que este método es escalable?

 

[Jesse_Pinkman_]

Debido al agua, cuando se congela, ¿de dónde deberían salir los cristales?
La nevera normal puede funcionar, pero tengo mi comida dentro y no quiero limpiarla cada vez.
Realmente he intentado muchas maneras de llegar al producto final y también desperdiciado una gran cantidad de disolventes y 2b3c también, pero la forma en que he descrito trabajado para mí mejor que los otros intentos.
Casi me confundí de todos los métodos diferentes, todo lo que diferentes pequeños cuencos con diferentes mezclas estaban de pie por todas partes, yo siempre miraba, que uno se desarrolla bien y que no.
Por ejemplo, cuando pones ipa helada al agua/polvo de cristalizacion, obtienes algunos cristales blancos instantaneamente pero no son claros y solo un poco, sp tienes que cristalizar de nuevo y el resto tiene que evaporarse, mira la ultima foto.
Las otras 3 fotos muestran lo que le pasa al rm en mi congelador, se convierte en una masa sólida que se funde a temperatura ambiente, pero sin cristales.

 

[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

 

[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 ?

 

[SunDay]

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