My 3-CMC synthesis

[draconic123]

Why does my 3 cmc oil turn black during acidification? i get it exactly 5.5-6 and it turns black

 

[Jesse_Pinkman_]

Maybe drop acid too fast...better cool the rm and the acid. Do you acidify the organic layer or with water together?

 

[draconic123]

i also forgot to mention that i used 10/100ml mix of hcl 36% and acetone to acidify i guess its either acetone or me adding acid to quickly... because at first it had rather nice color then went dark all of a sudden

 

[Jesse_Pinkman_]

I do not use acetone/hci mix, just 37% from freezer with dripping funnel, every 2-3 seconds 1drop...maybe you try this way one time

 

[UWe9o12jkied91d]

dcm only or with acetone?

 

[Jesse_Pinkman_]

As solvent for 2b3c i used dcm or ethylacetate, i tried both with similar results...

 

[UWe9o12jkied91d]

i meant for precipitation

 

[Jesse_Pinkman_]

I dont know what you mean? Which precipitation?

 

[draconic123]

Ok I know its dumb, however just to be clear, so after acidification you take top layer or bottom layer to dry using dcm? Im confused

 

[Jesse_Pinkman_]

I
only water layer

 

[UWe9o12jkied91d]

x

 

[Jesse_Pinkman_]

Dropped acid too fast, ph went down i think

 

[UWe9o12jkied91d]

No, I just evaporate forcefully, I will show u once filtered, they are primo

 

[UWe9o12jkied91d]

.

 

[Jesse_Pinkman_]

Looks good, how do you recrystallize now? Which amount water/ipa/acetone or do you use only water or only methanol?

 

[UWe9o12jkied91d]

If I can achieve crystalization after reaction I filter, dey and recrystalize from water/IPA. I don’t really have a ratio since I evaporate on heat anyways

 

[Jesse_Pinkman_]

Hmmm, and how do you want to get them clear?

 

[Jesse_Pinkman_]

I also had some issues to get them like this, but i think this is how they should look like...

 

[Jesse_Pinkman_]

And this takes some time, i did not reach this result in fast evaporating...but i am no expert, so maybe there are different methods

 

[draconic123]

I think I figured out why my acidification doesn't work lol, i've been adding acid through metal funnel, so acid musu have reacted with metal before going in to 3cmc freebase, therefore reaction was off, is that possible?

 

[Jesse_Pinkman_]

Better use glass funnel, metal is no good choice

 

[iheartamines]

A few other things that may have cause it to fail.

1. You have too much unreacted precursor 2b3c, which is what is turning your rm dark black/purple
2. If you are working on the organic layer, you haven't added enough ice cold Acetone. Add 2.5 times the volume of your reaction mixture.

 

[xoxoxoxo]

he dont need acetone.