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?

 

[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.

 

[draconic123]

I have tried out the reaction with ethyl acetate, and so far so good the color is Orange as described, however what concerns me is that after second washing layers of water flipped and was on top with acetate.. is it ok?

 

[Jesse_Pinkman_]

Never saw or heard about that, makes no sense to me...but If it is how you say, take the the organic layer, but fresh water and start acidification.

 

[Jesse_Pinkman_]

It is not possible, that ethylacetate mix with water, when doing this synthesis, water is at the bottom and organic layer is on top. Sometimes you need to wait some time, till they separat properly.

 

[draconic123]

i tried the reaction with ethyl acetate 5 times, i dont know why but 3 times the organic layer after methylamination was quite small and after first washing the organic layer sunk down, maybe the reaction was too hot and ethyl acetate evaporated, or i added to little of it.. quite strange

 

[draconic123]

other 2 times the reaction was fine

 

[Jesse_Pinkman_]

How much ethylacetate did you use for how much ketone and how long did you for reaction?

 

[draconic123]

50 ml 2b3c, 150 ml methylamine and 150 ml ethylacetate 25 mins to be sure. before the washing the synthetic layer was 2/3 of water layer. after washing it was all messed up organic layer didnt want to sink, and in the end it sunk to the bottom