My 3-CMC synthesis

[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?

 

[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

 

[Jesse_Pinkman_]

Hmmm... that's really strange.
Used destilled water?

 

[draconic123]

Yea, with sodium bicarbonate how you described in your post.

 

[Jesse_Pinkman_]

10%, 350ml, 35g Soda?
Maybe try less, 200ml .

 

[Jesse_Pinkman_]

Which kind of glassware did u use.
How separate the layers?
If it wont work at all, use a different solvent

 

[draconic123]

well the thing is it worked for 2 times so it must be something i've done wrong a couple of times which im trying to figure out what. for rm im using glass similar to yours in your post, for seperation i pour everything into separatory funnel , let it percipetate and drain

 

[draconic123]

for how long you mix 2b3c with ethyl acetate before pouring in methylamine?

 

[Jesse_Pinkman_]

Only a few minutes, then put all methylamine at once, seal the glass.
You can try this.
Remove the water layer after Amination first, then put water/Soda into organic layer, use 100ml/10g.
Shake and stirr a short time, then wait some time until the layers are proportional to their volume.
Remove water and wash 1-2 times also with just 100ml dest water, but still shake and stirr.
Sometimes it took some while separating until all water came from upside to bottom.
Normaly there should be no issues with that at all.

 

[Jesse_Pinkman_]

Ah, because the ratio
50ml 2b3c weights 75g,
please use 225ml ethylacetate, 150ml only double from 2b3c, better 3 times more

 

[draconic123]

I adjusted the ratios and everything went very smoothly, as described in your tutorial, one question though how long till crystals actually appear? Or atleast there is a hint of them so i would know that i succeeded

 

[Jesse_Pinkman_]

Nice to hear that it was just a ratio problem...
When acidification is done, take the water layer and let it evaporate by air, time depends on size of the bowls, you can use several small or one big with 1-2cm height of liquid.
Can take 2-3 days, up to 1 or 2 weeks, depends also on climate conditions, Air circulation, humidity etc.
There is no concrete answer i can give. In my environment mostly begins at day 3.

 

[draconic123]

tbh it was all ratio problem all along, when i tried it with dcm, i used to put 50g of 2b3c 100g methylamine and 150 g of dcm which is again wrong because it was supposed to be 100ml methylamine and 150 ml dcm... so many wasted reagents wow. there was always excess of non reacted 2b3c in rm

 

[draconic123]

First crystals, thanks alot guys for your patience with me