My 3-CMC synthesis

[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_]

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]

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

 

[draconic123]

After washing dirty 3cmc powder with acetone and recrystallizing with 1:2 water acetone mixture all i've got is white goo like substance and no crystals forming, any ideas?

 

[Jesse_Pinkman_]

That happens when you have moved the container and the solution came in motion, Just let it stand there for a few days and wait.

 

[draconic123]

ive got a question about ethyl acetate, when i did the reaction with DCM, the crystals turned out to be quite clean and the resulting weight was quite good aswell, however with ethyl acetate, it seemed like there still was unreacted 2b3c, im unsure whether i have to put in more solvent or methylamine, but the crystals came out really dirty and oily using ethyl acetate. do u guys have any opinions?

 

[Bazooka90]

The boiling point of ethyl acetate is 77°celsius.what temperature did u set?

 

[Bazooka90]

The boiling point of ethyl acetate is 77°celsius.what temperature did u set?

 

[Athanasias]

@Jesse_Pinkman_ thank you so much for contributing all of the information. It was of great benefit to me on my first attempt with 4mmc. I used 2b4m(50g), EthylAcetate and methylamineHCL. It was a small run as I didn’t want to waste. I yielded around 45%.
Overall, I’m very pleased and look forward to fine tuning everything. Thanks again!

 

[shoptilpop3x]

What other methods are out there to make molly, any alternative ways you suggest? What method is more possible and accessible for usa geography. Its difficult to order from sites who keep asking for business information.. I've heard of 2b3chl is there a way to obtain this product to make molly