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Unknown goodie and zinc

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DiMoiTou

DiMoiTou

Rising Star
Hi guys!

Yesterday, I was browsing through my goodies' stash and saw that my DMT wasn't as white as it used to be. I should have stored it in glass rather than cheap permeable plastic bag...
Anyway, I remembered about the zinc process to convert NMT back to DMT, so I thought I should give it a go.
I had two bags of DMT, same weight more or less, but not looking the same.. one was more flaky silvery pinkish and the other more pasty yellowish.
I poured each bag in a glass, covered in Hcl and added same weight of Zinc powder.
Stirred a bit and let it rest for the night.
And now, the two liquids don't look alike. One is clear while the other isn't. The cloudy one contained some yellowy orange stuff when I checked this morning. It dissolved/disappeared when I stirred.
My question is: have I done something wrong? Should I proceed in a different way from now on?
Perhaps one of the bags contained freebase and the other fumarate... Labels have faded, for I haven't touched the stuff in two years or so...:oops:

Thanks for your help!
 

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I started working with zink too recently, this looks like a synchronicity.
First, it's to convert spice-oxide to NN , not NMT to NN, but I guess you know and that was just a typo-thinko thingy.
Second, the wiki says using of vinegar, not HCL. I have no idea how that makes a different, I hope some chemical wizard chimes in to say something wise about that difference, or no difference.
Sorry I cant really help you further in your case, I have to examine my first results soon and hope to report.
Keep cool 8)
 
What Jees writes: zinc-mediated reduction (tentatively) reduces dmt N-oxide to dmt, not methylates nmt to dmt. I write "tentatively" because it is not clear if the reduction actually works, or if there is only a cleanup happening due to the A/B extraction that is part of the procedure, during the workup of the results. In the case of OP, it is unknown how much dmt has actually got oxidized and how much has not. I don't think that dmt salts can form N-oxides, so if fumarates are involved, zinc reduction would not work anyway.

Using dilute HCl instead of acetic acid should not make a difference, I think. But I am not a chemical wizard, so I might be wrong. In any case, I would not pour concentrated HCl onto dmt, the molecule might not like strong acids.

DiMoiTou: I think that the zinc mediated reduction needs a molar excess of zinc and strong stirring in order to work properly. The excess zinc is probably not an issue here, if I am correct that only a small portion of dmt has oxidized anyway. But the stirring does seem to be important.
 
Thanks for the answers. I googled before starting and read somewhere that Hcl is okay to use. I assume that the acid being stronger, the process is faster..
Sorry about the mix up between DMT-oxide and NMT.. It's been a while as I said. ;)

Am I right to assume I should keep the zinc in there for as long as it keeps bubbling?

I forgot to mention in my first post that the cloudy solution gets more clear when the orangey stuff (plant oils?) separate, after a while, but not as clear as the other one.

For now, I'll keep on stirring!😁
Cheers
 
Zinc has something of a tendency to form complex ions. This may or may not be an issue here with respect to relative efficacy of Zn/HCl vs. Zn/HOAc. The process is altogether unclear, we don't even really know what substance is behind the discolouration.
 
He had success with the zinc:

there is this supposedly very old mimo bark with a ton of supposedly oxidized material.
A very consistent result yields 50% good looking deems, and the other 50% (in weight) drops out as a very heavy orange oil on the bottom at room temp (before cooling/freezing). After freezing it looks like this:
resource.ashx

Together they come as 1.7 to 2 %

The orange is nothing short in activity, but it just annoys the process, it looks like heavier molecules with a higher vape temp, and it refuses to dissolve in naphta unless it is hot-to-boiling and low in saturation. It also dissolves slower in vinegar than the regular deems. In short a bit of a bugger to work with, it extracts more difficult, toluene is your friend to take it by the tail when making pulls on the bark.

The expectation was it to be oxidized nndmt, so zinc and vinegar was thrown at it.
From the 1.25 gr of the deep orange stuff, it delivered 0.695 gr of perfect looking deems just like on the right. That confirms something. So there was still a little puddle of yellow oil left that did not made the reduction process fully, or is other stuff than oxidized deems all together.
This oil is again hit by vinegar and zinc to see what comes of it. He is curious.
 
So this little puddle of deep yellow oil that did not made the reduction fully in the 1st attempt (well at least it went from deep orange to deep yellow) was subjected to a second hitting with vinegar + zinc and in the end dropped in a ml of HCL.

Almost everything went into crystals 0.355 gr , but the bottom layer were very slightly yellow and a bit sticky, but perfect for the purposes.

Numbers:
started with 1.25 gr of deep orange wax.
Molar mass dmt-n-oxide 204.3
Molar mass nn-dmt 188.3 (is 92% of the oxide)
So there is potentially 1.25 * 0.92 = 1.15 gr
1 batch 0.695 + second batch 0.355 = 1.05 gr
So 100 mg got missing in action, or 8% of the initial deep orange wax.
Maybe some weight of the heavy wax was no spice oxide after all and the reduction process acted as a cleanup step for it.

Conclusions:

* in contrast to claims that spice-n-oxide is non soluble in naphtha: this should be seen relative as he was able to solve all of his deep orange wax into it, but the naphtha was very warm and very low in saturation. When cooling to room temp it starts to drop out as oil soon. It is correct that it will fail (generally spoken) in pulling on plant material. But a backsalting process with hot naphtha takes it, but more care is needed as the pressure goes up!

* if one has a substantial drop out of oil (during a re-X or) when the typical vessel is cooling before freezing, don't discard it but collect it. Maybe save/collect from different batches till one has enough to do a zinc reduction act, mind that 2 steps might be called for. He poor off the white naphtha for whiter crystals, but the remaining orange oil goes also in the freezer (naphta pored off completely) so its stays no liquid oil but ends as orange hard wax shreds after evap like in the pic.

* He doesn't mind crystals turning yellow over time, but when you encounter a ton of oxidized material in plant matter to begin with, it calls for action. If your first naphtha-pulls yield is low like 1% or less, consistently while your workflow is fine, chances are like it. With the bark not disposed off, hit it with toluene (or xylene) to get the other 50%.
He hasn't extracted leafs just like bark, but seems leaves can have 90%+ of oxidized material.

* in his test, 92% answered to the reduction process, 8% got missing. He thinks jimjam is mostly oxide.
 
Thanks for the feedback.😉
I wish I had been as lucky as yourself. So far, I only recovered 1/4th of the DMT I used.:cry:
Attached is a picture of what my soup looks like. There's a bit of emulsion but I doubt 5grams are hiding in there...
I'll try warm pulls and cross my fingers!
I read something about using Nacl to force the DMT out... I might give that a try.
Suggestions are welcome.:oops:
 

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Yes there's a ton of solids precipating when basing after the reduction process, solids that aint of our interests to use later.

If NaOH was used to base, it is the zinc hydroxide that forms.
If sodium carbonate was used to base, it's zinc carbonate that forms.
This is so whether vinegar or HCL was used to reduce. Shoot me if wrong pls.

But we are more lucky than people who try to reduce harmaline to THH, because the zinc hydroxide/carbonate will not go to the naphta that we use here. But yes it stays in the watery layer and makes a little mess and is white solids.

1/4th?
You material cannot be gone, just a matter of getting it back.
X my fingers too for you.
 
You can dissolve that Zn precipitate away with concentrated ammonia, although I was lucky and mine precipitated. The resulting white solids were washed with IPA (this was a while ago and further details are no longer available).

There's considerable possibility of adsorption of goodies with all that nitrogen-loving surface area of ionic zinc powder. It might be worth rinsing it through in some kind of percolator?
 
Hi there,
A few weeks later, I tried another pull on my (warmed-up) mix with warm naphtha, followed by 48-hours freeze precip. Yield: none! :cry:
I still have that Zinc-based paste in a glass (still paste-ish after a month of air drying) and the lye mix stored in a PEHD bottle. I tested the pH of the mix, it turned out purple, so I think I don't need to add any more lye to it. What's wrong then?! Are my goodies lost forever? I see some white powder at the bottom, could it be precipitated freebase? Why wouldn't my naphtha extract it? :|
Could the freebase be somehow trapped in the zinc paste?
Experienced chemists, please chime in!
Cheers!

PS: I don't have any ammonia, IPA or percolator :oops:
 
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