My 3-CMC synthesis

[antrax]

My 3-CMC synthesis:
at first i want to thank William Dampier for his advices.

I use a sealed glass with a thick toppits foil between lid and glass to prevent fumes.
And no, it will NOT explode, if you use this kind of glass.
I tried with dcm and ethylacetate and both works fine.
The benefit of ethylacetate is the short cooking time, about 20 min.
You do not have to heat it till above 35 degress like with dcm.
But the layers are opposite, water down in ethylacetate and dcm up.
For example:
100g 2b3c
300 dcm
200 methylamin40% aqua
3 hours at aprox 36 degrees
20 min with ethylacetate
After that, open the glass and put same amount as rm, icecold,dest.water /10% sodium bicarbonate inside, this is the first wash to get rid of methylamine.
2 additional washing with dest.water
(same amount as rm)
extract both 2 last washings(water layer) with dcm to get rest of freebase,
then put into rm.
After that, add same amount fresh, cold dest.water into rm, let it stir some time.
Then separate organic and water layer.
I tried different kind of acidificaction.
organic layer alone and organic/water layer together.
I prefer the second one.
Organic layer will be disposed in this case.

put on magnetic stirrer
for acidificaction i use dripping or separatory funnel, drop by drop
(every 2-3 seconds)
till ph6, about 40ml 37% HCI
(i do not mix it with acetone)
While acidificaction the rm begins to change its color from yellow to orange.
After that, separate the water layer with a separatory funnel, put it into a bowl or dish, let it crystallize, this will take some time, 2-3 days.
Freezer gave me strange results so i do not recomend it.
After the crystals have formed, i had different results, sometimes very clear, sometimes light yellow.
So, to get them clear as possible, you have to crush them to powder, wash with acetone, filter with buchner.
Put the acetone into a bowl and let it evaporate, there will be some rest of powder mostly, that will be crushed and washed again.
The washed powder from buchner will be dried and we recrystallize it again.
300ml beaker, 1ml dest.water per 1g powder heated on magnetic stirrer till 60/70 degrees.
Then put Powder into the beaker, let it dissolve and stir 1-2 min.
Then put 2ml ipa or acetone per 1g powder into the beaker, let it stir a short time.
After that, put again into a bowl or dish, evaporate and crystals will form.
Repeat this step until you got the clearness which you want to have.

About the yield (aprox 30-40%, at first i only had about 20%, because i did not re-use the solution after crystalisation), to be honest, i expected more, but maybe my synthesis has some issues or something happened i do not know.
If someone has better experiences, please share your knowledge.
As far as i see here in the forum, many people have questions about 3-cmc but good and helpful answers are hard to find.

The pictures are from different batches and different stages.

Jesse_Pinkman_To measure pH do you use pH measuring strips or a digital pH measuring device?
For filtration, do you do it by gravity or by vacuum?
To separate two liquids of different density, do you use a separatory funnel?
During the methylamination process, did you close the container so that the fumes do not escape or did you leave it open?
To obtain transparent crystals, did you wash them or what technique did you use?
How many days did it take for the crystals to form and in which container did you leave them to rest and did you close said container or did you leave it open so that the solvent could evaporate?
How much did you pay for the precursor? and the precursor was already ready or you had to buy a pre-precursor and then synthesize the precursor yourself?
Thank you!!

 

[Jesse_Pinkman_]

To measure pH do you use pH measuring strips or a digital pH measuring device?
For filtration, do you do it by gravity or by vacuum?
To separate two liquids of different density, do you use a separatory funnel?
During the methylamination process, did you close the container so that the fumes do not escape or did you leave it open?
To obtain transparent crystals, did you wash them or what technique did you use?
How many days did it take for the crystals to form and in which container did you leave them to rest and did you close said container or did you leave it open so that the solvent could evaporate?
How much did you pay for the precursor? and the precursor was already ready or you had to buy a pre-precursor and then synthesize the precursor yourself?
Thank you!!

antraxI used a manual vacuum pump to filter via buchner

 

[UWe9o12jkied91d]

To measure pH do you use pH measuring strips or a digital pH measuring device?
For filtration, do you do it by gravity or by vacuum?
To separate two liquids of different density, do you use a separatory funnel?
During the methylamination process, did you close the container so that the fumes do not escape or did you leave it open?
To obtain transparent crystals, did you wash them or what technique did you use?
How many days did it take for the crystals to form and in which container did you leave them to rest and did you close said container or did you leave it open so that the solvent could evaporate?
How much did you pay for the precursor? and the precursor was already ready or you had to buy a pre-precursor and then synthesize the precursor yourself?
Thank you!!

antraxTo measure pH do you use pH measuring strips or a digital pH measuring device?
Paper and by smell/color

For filtration, do you do it by gravity or by vacuum?
gravity on muslim cloth/gauze

To separate two liquids of different density, do you use a separatory funnel?
Decant as much water as possible, leaving at least some residues

During the methylamination process, did you close the container so that the fumes do not escape or did you leave it open?
condenser without running water sealed gently with a glove and rubber band

To obtain transparent crystals, did you wash them or what technique did you use?
Precipitation -> Filtration -> Further recrystalization in water + acetone/IPA

How many days did it take for the crystals to form and in which container did you leave them to rest and did you close said container or did you leave it open so that the solvent could evaporate?
Depending on how big and pretty you want you crystals to be you can evaporate a given amount of solvent during re-x, more evaporation and quick cooling = small crystals but smokeable, less evap and gentle cooling = big ones If most solvent is evaporated crystalyzation can take less than an hour, open pyrex container

How much did you pay for the precursor? and the precursor was already ready or you had to buy a pre-precursor and then synthesize the precursor yourself?
No comment
Thank you!!
youre welcome

 

[lheartamines]

Be careful when using a digital ph device and DCM, if you leave it in the rm while monitoring it will melt the device.

 

[Jesse_Pinkman_]

Be careful when using a digital ph device and DCM, if you leave it in the rm while monitoring it will melt the device.

lheartaminesYes, i had this with a thermometer

 

[lheartamines]

I wonder what it is about 3-cmc that it seems it's preferable to work in the aqueous layer instead of the organic layer when doing acidification. I also tried your method @Jesse_Pinkman_ and had good results working the aqueous layer. When working the organic layer, I never get salt, just sludge. But I also am working with very small amounts of ketones, around 15 grams. I am trying to perfect my technique as an amateur and do not want to waste large amounts of valuable precursors.

 

[UWe9o12jkied91d]

I wonder what it is about 3-cmc that it seems it's preferable to work in the aqueous layer instead of the organic layer when doing acidification. I also tried your method @Jesse_Pinkman_ and had good results working the aqueous layer. When working the organic layer, I never get salt, just sludge. But I also am working with very small amounts of ketones, around 15 grams. I am trying to perfect my technique as an amateur and do not want to waste large amounts of valuable precursors.

lheartaminesIt has to do with the nature of the precursor

 

[ELAIGIBBOR]

Would love to try your synthesis, keep it improving brother

 

[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]

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

Jesse_Pinkman_only the organic layer, yes i suspect i acidify too fast.

 

[UWe9o12jkied91d]

only the organic layer, yes i suspect i acidify too fast.

draconic123haloketone turn black with acid, check reaction parameters

 

[Jesse_Pinkman_]

only the organic layer, yes i suspect i acidify too fast.

draconic123Put same amount dest.water into rm, then acidificaction drop by drop slowly, then take water layer to evaporate

 

[xoxoxoxo]

Put same amount dest.water into rm, then acidificaction drop by drop slowly, then take water layer to evaporate

Jesse_Pinkman_you get visible layers of water and freebase after adding acid??

 

[Jesse_Pinkman_]

you get visible layers of water and freebase after adding acid??

xoxoxoxoYes, and after that, take the upper layer, bottom layer will be disposed.

 

[Jesse_Pinkman_]

Yes, and after that, take the upper layer, bottom layer will be disposed.

Jesse_Pinkman_If dcm is used, when ethylacetate is used you take the bottom/water layer

 

[draconic123]

you get visible layers of water and freebase after adding acid??

xoxoxoxoI only get whole black liquid with no layers

 

[UWe9o12jkied91d]

I only get whole black liquid with no layers

draconic123He means IF you add water.

 

[Jesse_Pinkman_]

I only get whole black liquid with no layers

draconic123Then you do something wrong i think...would you like to describe your steps of your synthesis?

 

[draconic123]

Then you do something wrong i think...would you like to describe your steps of your synthesis?

Jesse_Pinkman_I carried out methylamination by leaving 2b3c dcm and methylamine for 12 hours no heat just stirring, disposed of top layer, washed bottom layer 2 times, disposed of top layer, added acid till 6, and the liquid became very dark red.

 

[UWe9o12jkied91d]

I carried out methylamination by leaving 2b3c dcm and methylamine for 12 hours no heat just stirring, disposed of top layer, washed bottom layer 2 times, disposed of top layer, added acid till 6, and the liquid became very dark red.

draconic123procedure 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.)

 

[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