Full recipe on 3 CMC?

[WooWater]

need help on making 3cmc crystal rocks

target:

 

[Heineken]

very easy to made

 

[blosuetoday]

Thanks for the help.

 

[Yavuz1453]

I tried so hard and it didn't workNo one helped me, but they should not forget that one day we will die, it's a lie world, I'm so sorry

 

[Yavuz1453]

 

[Jesse_Pinkman_]

so, my experience is,
100g 2b3c
300dcm
200methylamin40% aqua
3 hours stirring
I use a sealed glas 1,8l, put foil between lid and glass so that nothing smells or gas escapes.
After reaction took place
2 times washing with dest.water
1 time extract water phase with dcm
put into rm,
add same amount fresh water into rm
put on magnetic stirrer
acidificaction drop by drop till ph6, about 50-55ml HCI,
after that take the water layer,evaporate the, let it crystallize, takes some time
opt. rotovap till 50% of the water is gone, then air drop


ethylacetat is possible, takes only 20 min, no heating necessary, rest same prosedure like with dcm

I waited min 2 days untill crystals began to form, these on the picture have not been washed with acetone but after that they are like glass. Very nice

 

[WildDoc]

How much ethyl acetate per gram?

 

[Jesse_Pinkman_]

I did it with 1:3, like with dcm

 

[Jesse_Pinkman_]

Maybe there are other options but it worked for me

 

[Bazooka90]

 

[Bazooka90]

if we use ethyl acetate no need to heat?
need to shake for 20 minutes?

 

[Jesse_Pinkman_]

I used magnetic stirrer, did not try shake, but could be possible, i dont know

 

[Jesse_Pinkman_]

I used magnetic stirrer, did not try shake, but could be possible, i dont know