Моят синтез на 3-CMC

[mithyl2]

Това е страхотно.

Защо смятате, че фризерът ви е дал странни резултати по време на кристализацията?

Колко добре според вас този метод се мащабира?

 

[Jesse_Pinkman_]

Заради водата, когато тя замръзва, откъде трябва да се появят кристалите?
Нормалният хладилник може би работи, но аз имам храната си вътре и не искам да го почиствам всеки път.
Наистина опитах много начини да стигна до крайния продукт и също така изхарчих много разтворители и 2b3c също, но начинът, който описах, ми подейства по-добре от другите опити.
Почти се обърках от всички различни методи, всички тези различни малки купички с различни смеси стояха наоколо, винаги гледах коя се развива добре и коя не.
Например, когато сложиш леденостудена ипа към водата/праха за кристализация, веднага се получават някакви бели кристалчета, но те не са ясни и са съвсем малко, сп трябва да се кристализира отново, а останалото да се изпари, виж последната снимка.
Останалите 3 снимки показват какво се случва с рм във фризера ми, той се превръща в твърда маса, която се топи на стайна температура, но няма кристали.

 

[HerrHaber]

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

 

[xoxoxoxo]

Получавам 72 г кристали под формата на 2b3ch
и 76g кристална форма 2b4m.
е наистина лесно да се направи форма ме.
Същото 4mmc е по-добре като 3cmc
на 4mmc имам нормален сън и ядене, но на 3cmc е проблем 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