extracting n-oxide?

[JJ Spigglesworth]

Hi All

Ive recently completed an A/B on 400g MHRB.

3 x 1.5hr boil in 1.5L 3:1 H2O:Vinegar,
separate liquids, freeze solids for 12hrs,
final 3+ hr boil on thawed solids.
liquids combined (3+ L total) all reduced down to ~ 500ml.
Basified (200g NaOH in 200mL H2O added)
pulled with naptha (colemans camp fuel 5 x 200ml, last 2 pulled warm)
freeze precip
collect solids and rex from light naptha (distilled colemans)

My yield was much lower than expected, less than 1g from 400g bark!

I've noticed a larger proportion of yellow goo after reX which I'm presuming to be DMT-N-oxide, almost 1g of goo for my 1g of spice. The bark was roughly 6 months old so I'm thinking that much of the DMT has oxidised in the bark. I plan to go a zinc/Acetic acid reduction on the goo so I want to collect it all.

Here's my questions:

Is N-oxide extracted in the same way as DMT? e.g. Do I need to process the bark further in order to extract all the N-oxide? (lower pH/ longer boil perhaps)

Is there a better solvent for N-oxide than naptha? naptha is clearly a poor solvent for N-oxide as the oxide is left behind during reX. perhaps xylene / toluene would pull N-oxide along with jungle alks?

What is the best method for cleaning the goo ready for reduction? is it even necessary to clean it up or should I presume it is 100% N-oxide for the reagent calculations for reduction.

Thanks for reading, hope you can help!

 

[Ambivalent]

the oxides of dmt are extracted in the same way as dmt. basify till Ph 10-12, and pull with non polar solvent.

but as you mentioned, you need a little bit more polar solvent than naphtha or hexane, like limonene xylene, or dcm.

and the easiest method in my head for cleaning the converted N,N would be, to first make the reduction, than make a small a/b on that solution with naphtha and you should get only dmt out, if the reduction went ok.

there is a tek on reduction with zinc, you can find it in the wiki. follow that and post your results.

 

[Parshvik Chintan]

there is a tek on reduction with zinc, you can find it in the wiki. follow that and post your results.

afaik you can add zinc dust to any acid step and proceed with the tek from there.

 

[Ambivalent]

there is a tek on reduction with zinc, you can find it in the wiki. follow that and post your results.

afaik you can add zinc dust to any acid step and proceed with the tek from there.

yes, i am not saying you cant. but in the situation of JJ Spiglesworth he already has crude extract, so i was explaining how to proceed from there.

 

[JJ Spigglesworth]

Hi Guys thanks for your replies

there is a tek on reduction with zinc, you can find it in the wiki. follow that and post your results.

Yes I plan to carry out the zinc/Acetic acid reduction from the wiki. I have done this before with good effect, converting 200mg yellow goo to around 150mg of the whitest freebase I've ever seen.

afaik you can add zinc dust to any acid step and proceed with the tek from there.

I'm not sure If it's a good idea to add zinc just to the acidic mimosa tea. although it would no doubt convert N-Oxide to DMT, there will be numerous other reduction reaction going on alongside which will not only use up the zinc but could produce unknown (possibly toxic) products.

Whilst I source some zinc, I decided to carry out an experiment on my goo. I dissolved it in hot vinegar, filtered, basified, extracted 3x with light naptha. this created 3 layers
bottom (aqueous)
middle (yellow N-oxide goo)
top (organic)
The organic layers were combined, evapped till coudy and freeze precipitated to give an extra ~100mg of freebase that was 'trapped' in the goo!
The yellow layer was collected, and this now solidifies into a yellow / orange waxy solid. perhaps this is mostly plant fats now? I guess only a zinc reduction will tell.

 

[Silly(c)One]

Congrats on your last experiment, nicely played
I wouldn't say it's plant fats before testing with zinc. I've had both good and bad surprises on "oily stuff" from my extractions on MHRB.
If you have access to chloroform, I was told by a professional chemist that it's a great solvent to get n-oxide from your bark solution... More efficient than naphtha and heptane/hexane for that purpose. You have to evap it all the way though, no cold precip with that one.