failed FASA (update)

[BioBoostedSpirit]

Hello buds, i wanted to post this in FAQ section but there is no "new topic" mark on the upper right corner for me, sorry in the case of posting in wrong section..

So yesterday i tried my first FASA experiment witch turned not as expected and i was wondering if someone can explain why this is happened.
Long story short: i baked some epsom salt in an oven at 210 celcius till it formed a hard cake, poulverised it with a mortar and added some to 200 ml of acetone. Mixed it well and after filtered it in a funnel filled with cotton.
After i took 310mg of fumaric acid (my fumaric acid is over expiration date, idk if it counts but some buds in the chat told me its fine) and added it to 50 ml of warm acetone,stirred it well until totally dissolved.Also 1000mg of dmt were added to 50 ml of warm acetone in different container and stirred well. Right after i added fasa in the container with dissolved dmt and stirred it well while its warm. (I read that mixing those two should make a reaction and an precipitate should come out right away, but in this step i observed nothing, the solution stayed clear)
In hope do make something out of it i decided to freeze precipitate the solution.After 12 hours i took out the pyrex dish from the freezer and was really amazed(i never saw such big ,shardlike long crystals whitch formed on the bottom). I poured out the acetone and let the dish to dry.But after very short time i saw that all those crystal are melting X) , until everything became a colorless substance(which i believe is dmt)
Anyway,what do you guys believe? I will try adding some warm naphtha in container with melted substance in hope to save and re x the dmt and will see what happens. But why my FASA failed?

Big thanks in advance buds
Best regards

 

[endlessness]

On a phone here, will try to type well...


To make fasa,you saturate the acetonr, so add more fumaric acid, that way you make sure all your dmt will react with the fumaric. Excess fumaric acid will stay in solution so no worries.

Also, never stir after adding fasa to your dissolved dmt,instead you want to add your fasa as slowly as possible, dropwise, and let it precipitate slowly, that way you have nicer stable crystals.

Now what i would do if i were you is try to let that clear aubstance dry, it might still crystalize, it could be moisture that dissolved your fumarates.

Id also get your fasa+dmt acetone and evap it all to see if you have anythi g left there. Id put it all togwther if it is t solid yet, make paste with sodium carb and bit of water, let dry, pull with dry acetone and do propper fasa this time.

Using naphta to what you have wont work because dmt fumarate isnt soluble in naphtha, only freebase is

.

Hello buds, i wanted to post this in FAQ section but there is no "new topic" mark on the upper right corner for me, sorry in the case of posting in wrong section..

So yesterday i tried my first FASA experiment witch turned not as expected and i was wondering if someone can explain why this is happened.
Long story short: i baked some epsom salt in an oven at 210 celcius till it formed a hard cake, poulverised it with a mortar and added some to 200 ml of acetone. Mixed it well and after filtered it in a funnel filled with cotton.
After i took 310mg of fumaric acid (my fumaric acid is over expiration date, idk if it counts but some buds in the chat told me its fine) and added it to 50 ml of warm acetone,stirred it well until totally dissolved.Also 1000mg of dmt were added to 50 ml of warm acetone in different container and stirred well. Right after i added fasa in the container with dissolved dmt and stirred it well while its warm. (I read that mixing those two should make a reaction and an precipitate should come out right away, but in this step i observed nothing, the solution stayed clear)
In hope do make something out of it i decided to freeze precipitate the solution.After 12 hours i took out the pyrex dish from the freezer and was really amazed(i never saw such big ,shardlike long crystals whitch formed on the bottom). I poured out the acetone and let the dish to dry.But after very short time i saw that all those crystal are melting X) , until everything became a colorless substance(which i believe is dmt)
Anyway,what do you guys believe? I will try adding some warm naphtha in container with melted substance in hope to save and re x the dmt and will see what happens. But why my FASA failed?

Big thanks in advance buds
Best regards

 

[downwardsfromzero]

i took out the pyrex dish from the freezer and was really amazed(i never saw such big ,shardlike long crystals whitch formed on the bottom). I poured out the acetone and let the dish to dry.But after very short time i saw that all those crystal are melting

Sounds to me like your acetone was still damp. Is it very humid where you are? Also, using warm acetone with magnesium sulfate increases the chances of condensation reactions of the acetone itself. These reactions generate water.

Either dehydrate cold or use sodium sulfate or calcium sulfate for dehydration instead. They are much weaker Lewis acids and thus much less prone to catalysing condensation reactions in the acetone.

 

[BringsUsTogether]

Hello buds, i wanted to post this in FAQ section but there is no "new topic" mark on the upper right corner for me, sorry in the case of posting in wrong section..

I think this happens after you become a full member. I can't post in the new member section either.

 

[BioBoostedSpirit]

Buds,a thousand thanks to you all for taking your time and responding.

All your tips are highly appreciated ,and im working with them a.t.m.:thumb_up:

Let love & light be with you

Best regards

 

[BioBoostedSpirit]

Once again greetings everybody !!

Here are some results of the final product.
Actually i did nothing special, just waited (as endlessness said) until the substance is dry, and it indeed crystallized. Looks like the problem was moisture after all. The final product is slightly yellow,white crystalline powder witch i believe*(this is my first time dmt fumarate making experiment, so it whould be nice of you buds if you told me if it looks like dmt fumarate ,and if this form is ready for consumption)* is dmt fumarate. Apperance of the substance as also its condensation is totally different from dmt freebase, should i say more stable looking substance ? I used 1000mg dmt freebase in this experiment and the final product yelded around 1200mg.

Here are couple of pics:
A pyrex dish with crystal forming and an pyrex dish cap with some crystalline powder and with some big yellowish crystal chunks. After those yellow crystal chunks are powdered they became crystalline powder also.

Big thanks to you buds

Thanks for watching

 

[BioBoostedSpirit]

And my last step..
I finally decided to clean my fumarates with IPA method as folks saying in "cleaning up dirty fumarates" thread.
I carefully dissolved everything in boiling hot 99.5% IPA (it took me a while), filtered through a funnel with a small piece of cotton in it and placed my pyrex dish in the freezer over night. Freeze precipitation did not worked for me, when i took my dish out of the freezer nothing precipitated. So, i waited till everything is evaporated and was left with crystalline mass and some small salt like crystals on the bottom. Final yield was around 1100mg of slightly yellow white crystalline powder.
Next time will do whole FASA procedure with your tips buds, once again thanks for posting:thumb_up:

Looking forward to try some of the fumarate i made

Best regards everyone

 

[some one]

Sounds to me like your acetone was still damp. Is it very humid where you are? Also, using warm acetone with magnesium sulfate increases the chances of condensation reactions of the acetone itself. These reactions generate water.

Either dehydrate cold or use sodium sulfate or calcium sulfate for dehydration instead. They are much weaker Lewis acids and thus much less prone to catalysing condensation reactions in the acetone.

I didn't know this. So best to place the bottle of aceton + mag sulph in a fridge while it dehydrates? After the reaction is done, can it be brought back and stored at room temp with the mag sulph still in it?

Is there a disadvantage of using Sodium/Calcium Sulphate instead of Magnesium Sulphate? What about Calicium Chloride?

 

[downwardsfromzero]

It's really only of consequence if you need/want ultra-pure acetone (in which case, probably do something else). I don't know how quickly the reaction occurs but it's best to use your acetone fairly soon after the dehydration as it will keep absorbing water from the atmosphere anyhow.

I just wouldn't leave acetone standing over MgSO4 in a warm place for any great length of time, personally.

Calcium chloride can't be used to dry acetone (it's soluble or something?) and sulphates of sodium and calcium just work a bit slower than MgSO4.

 

[some one]

Great info, thanks