Moja sinteza 3-CMC

[mithyl2]

to je odlično.

zakaj mislite, da je zamrzovalnik med kristalizacijo dal čudne rezultate?

kako dobro se po vašem mnenju ta metoda skalabilna?

 

[Jesse_Pinkman_]

Zaradi vode, ko njena voda zmrzne, od kod naj bi prišli kristali?
Običajni hladilnik morda deluje, vendar imam v njem hrano in ga ne želim vsakič čistiti.
Res sem poskusil zelo veliko načinov, da bi prišel do končnega izdelka, in tudi zapravil veliko topil in 2b3c, vendar mi je opisani način deloval bolje kot drugi poskusi.
Skoraj sem postal zmeden od vseh različnih metod, vse te različne majhne posodice z različnimi mešanicami so stale naokoli, vedno sem gledal, katera se dobro razvija in katera ne.
Na primer, ko v kristalizacijsko vodo/prah daš ledeno hladno ipo, takoj dobiš nekaj belih kristalov, ki pa niso bistri in jih je le malo, sp moraš ponovno kristalizirati, preostanek pa mora izhlapeti, poglej zadnjo sliko.
Ostale 3 slike prikazujejo, kaj se zgodi z rm v mojem zamrzovalniku, postane trdna masa, ki se pri sobni temperaturi topi, vendar brez kristalov.

 

[HerrHaber]

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

 

[xoxoxoxo]

dobim 72 g kristalov oblike 2b3ch
in 76 g kristalov oblike 2b4m.
je resnično enostavno narediti obliko me.
enako 4mmc je bolje kot 3cmc
na 4mmc im normalno spanje in jesti, ampak na 3cmc je problem 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