My 3-CMC synthesis

[antrax]

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_]

I 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?
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_]

Yes, 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]

It 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_]

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

 

[draconic123]

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

 

[UWe9o12jkied91d]

haloketone turn black with acid, check reaction parameters

 

[Jesse_Pinkman_]

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

 

[xoxoxoxo]

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

 

[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]

I only get whole black liquid with no layers

 

[UWe9o12jkied91d]

He means IF you add water.

 

[Jesse_Pinkman_]

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

 

[draconic123]

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]

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.)

 

[draconic123]

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_]

I
only water layer