My 3-CMC synthesis

[mithyl2]

this is great.

why do you think the freezer gave you strange results during the crystallization?

how well do you think this method scales up?

 

[Jesse_Pinkman_]

Because of the water, when its freezing, where should the crystals come from?
Normal Refrigerator maybe works but i have my food inside and dont want to clean it everytime.
I really tried very much ways to get to the final product and also wasted a lot of solvents and 2b3c too, but the way i described worked for me better than the other tryouts.
I almost became confused from all different methods, all that different little bowls with different mixtures were standing all around, i always watched, which one develops good and which not.
For example, when you put icecold ipa to the crystalization water/powder, you get some white crystals instantly but they are not clear and just a little bit, sp you have to crystallize again and the rest has to evaporate, look last picture.
The 3 other pictures show what happens to the rm in my freezer, it becomes a solid mass which melts at room temperature, but no crystals.

 

[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