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_]

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

draconic123Maybe drop acid too fast...better cool the rm and the acid. Do you acidify the organic layer or with water together?

 

[draconic123]

procedure sounds good, drip slower with good stirring
also be patient with just DCM, sometimes it decides to crash out in 2 min, sometimes it needs an hour stirring, acetone will help here I advise to use it (cold if poss.)

UWe9o12jkied91di 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 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

draconic123I 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]

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

Jesse_Pinkman_dcm only or with acetone?

 

[Jesse_Pinkman_]

dcm only or with acetone?

UWe9o12jkied91dAs solvent for 2b3c i used dcm or ethylacetate, i tried both with similar results...

 

[UWe9o12jkied91d]

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

Jesse_Pinkman_i meant for precipitation

 

[Jesse_Pinkman_]

i meant for precipitation

UWe9o12jkied91dI dont know what you mean? Which precipitation?

 

[draconic123]

I dont know what you mean? Which precipitation?

Jesse_Pinkman_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_]

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

draconic123I
only water layer

 

[UWe9o12jkied91d]

x

 

[Jesse_Pinkman_]

x

UWe9o12jkied91dDropped acid too fast, ph went down i think

 

[UWe9o12jkied91d]

Dropped acid too fast, ph went down i think

Jesse_Pinkman_No, I just evaporate forcefully, I will show u once filtered, they are primo

 

[UWe9o12jkied91d]

Dropped acid too fast, ph went down i think

Jesse_Pinkman_.

 

[Jesse_Pinkman_]

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

 

[UWe9o12jkied91d]

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

Jesse_Pinkman_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_]

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

UWe9o12jkied91dHmmm, and how do you want to get them clear?

 

[Jesse_Pinkman_]

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

UWe9o12jkied91dI also had some issues to get them like this, but i think this is how they should look like...

 

[Jesse_Pinkman_]

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

UWe9o12jkied91dAnd 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_]

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?

draconic123Better use glass funnel, metal is no good choice

 

[iheartamines]

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?

draconic123A 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]

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.

iheartamineshe dont need acetone.