Attempt at Dmt-oxide reduction

[Synkromystic]

These experiments are to document an attempt at a reduction of dmt-oxide using zinc powder and hcl. **An assumption has been made that the sample contains at least a small amount of Dmt-oxide.

The dmt is from Mimosa Hostilis. It was collected from a Freeze precipitation of Crown Naphtha from an A/B extraction. All pulls were mixed together.

Sample A – Original sample 2.5 grams. Kept as is, for a control
Sample B – Starting sample 2.5 grams. Dissolved in hcl/ water mix and based with Naoh. Pulled with very hot Bestine. Left to cool slowly and then freeze precipitated.
Sample C – Starting sample 2.5 grams. Reduction Sample. Dissolved in hcl/water mix. Zinc Added. Filtered and Based with Naoh. Pulled with very hot Bestine. Left to cool slowly and then freeze precipitated.
Sample D – Starting sample 2.5 grams. Dissolved in very hot Bestine. Freeze precipitated.

1st image - All the samples together. They are slightly waxy orange crystals for the most part.

2nd image - Sample B and C after dmt added to hot hcl/water solution.

3rd image - Zinc Reduction on Sample C

4th image - After zinc was filtered from Sample C

5th image - Immediately after adding Naoh to base. The camera is not the best, but Sample C is slightly whiter than Sample B

6th image - After pulling with hot bestine. Difficult to see, but Bestine is still in the Sample C jar. Sample D is on the left. C is in the middle. B on the right.

7th image - On sample C, the reduction sample, there was some residue leftover at the bottom of the jar after pulling with bestine. There is a picture attached, but it's rather difficult to see. The residue is very slightly greyish in color, but acts much more like dmt than zinc. It will not go into the bestine solution no matter how hot the bestine gets. **** Recently I have done a few different ''reductions'' on the same batch of orange dmt. This residue has occurred on each experiment. It will re-dissolve in an hcl solution, and will come out when based with naoh again, but it will not dissolve into bestine, or 90% ipa. It looks and acts like dmt with a slightly gray color.

A reaction clearly took place once the zinc was added to the warm mix of hcl/water and dmt. The solution went from dark orange to almost clear within a minute after the zinc was added.

Sample C, the reduction sample, has produced the most shiny clear crystals, and the least amount of impurity at the bottom ( I am assuming it is plant oils, or the reduction did not get completed 100%)

All samples were left to cool very slowly. Room temperature was reached after 4 hours, and then into fridge temperatures for about 2 hours. Then into the freezer for about 4. I have grown beautiful crystals doing this before, but maybe the solvent wasn't as saturated as it could be, so I had to freeze preicp to get most of the crystals out.

I cannot comment on the exact yield at this time.

 

[endlessness]

Interesting

Seems a re-a/b was as effective in 'cleaning it up' as the zinc reduction. But gotta wait for yield results. Hard to know if there was any n-oxide in the first place there. If so, then we'd expect higher amounts in the zinc reduction group. Keep us informed!

Thanks for sharing the experiment results!

 

[Synkromystic]

Concerning yields. The yield numbers are based off recoverable white crystal. So unfortunately they will not be exact, as I was not able to separate all of it from the oil at the bottom of the jar very cleanly. I estimate that I recovered around 90% of the white crystal in Sample C (reduction) and sample B (acid/base)

Sample B (Acid/Base) 1.4 grams of very white crystal recovered. 56 %
Sample C (Reduction) 1.2 gram of the cleanest crystal I have ever seen. 48 % *** Note I have done this reaction a couple of times very recently with 10 and 20 grams starting material(from same batch) and I have recovered around 60 % of nearly as clean spice as Sample C (could be the same purity but got crystallized differently)

Considering the analysis’s that have been done regarding the oxide content in mimosa, and how there has been little to no oxide found... I don't think it is possible to make a clear judgement with this experiment how much n-oxide was in the sample in the first place. I think there's too many places to ''lose'' product. I tend to the ''superficial oxidation'' hypothesis. That there is only a minute amount of n oxide, but it's presence has a much greater effect on the whole consistency and color of the dmt. So I think it's deceiving how a little bit of oxide can effect the whole.

The color change of the hcl solution in sample C after the zinc was added is what fascinates me the most. From orange to grey to almost clear.

On sample B (acid/base only), after base was added and very hot bestine was pulled, there was a bright orange layer between the water and the bestine that would not go into the solvent. Yet for sample D which the same product, all of the oil went into the bestine. Is it possible that some of the ''oil'' felt a greater attraction to the water, and just didn't want to let go so it didnt go into the bestine?

On the reduction sample C, there was quite a bit of slightly grey sediment that would not dissolve in bestine, or in ipa. Any ideas on what that is? I did a separate acid/base and it would dissolve in hcl and re emerge upon adding Naoh. It looked like dmt with a little bit of zinc attached to it...is this possible?

I find interesting the amount of impurity in D vs C vs B. C having the least, but was the lowest yield, but not by much.

 

[Orion]

The color change of the hcl solution in sample C after the zinc was added is what fascinates me the most. From orange to grey to almost clear.

Zinc must do something afterall, but what? Maybe it grabs something from solution, or maybe it simply takes the colour out with impurities still present in solution ? Totally guessing here, but very interesting.

Perhaps some coloured impurities stick to the zinc? A similar thing happens in solvents when washing pigment from brushes. Sometimes a pigment will dye the solution, which can stay for weeks until another pigment is mixed in. The next day there will be sediment and much clearer solution. I think something similar might be happening here? The zinc is causing some of the impurities to stick to it and join the sediment ?

Your C pile also has the most vitreous lustre which leads me to think there's even less impurities matting out the surface. Another a/b on the B sample would likely get you the same, but looking at sample C it looks like you saved some effort there.

 

[downwardsfromzero]

On sample B (acid/base only), after base was added and very hot bestine was pulled, there was a bright orange layer between the water and the bestine that would not go into the solvent. Yet for sample D which the same product, all of the oil went into the bestine. Is it possible that some of the ''oil'' felt a greater attraction to the water, and just didn't want to let go so it didnt go into the bestine?

The difference is in the latter case there is no water. The orange oil is soluble in either water or Bestine but appears to form a separate phase, presumably the oil + a small amount of water and maybe a tiny amount of something from the Bestine, which is then essentially insoluble in either salty water (NaOH + HCl = NaCl i.e. salt), or Bestine.

Zinc must do something afterall, but what? Maybe it grabs something from solution, or maybe it simply takes the colour out with impurities still present in solution ? Totally guessing here, but very interesting.

Zinc salts could certainly form insoluble complexes with whatever the coloured material is. We could do with working out what the orange oil really is and also analysing the zinc-containing residue.

From the photos, it looks as though the yields may have been affected by spillage?