Oh past self did you not read anything?!


Am I right in saying these alkaloids are so delicate even acetone oxidises them?
Also, when the freebase is dry will sodium carbonate be a contamination?

No, harmalas are far from delicate - it is that there is not a good, readily available solvent to pull them. DCM works but is not excellent. Naphtha, limonene, xylene etc all dissolve freebase harmalas very poorly.

Precipitating them out of basic solution is really a superior approach to isolate harmalas.

Hi, did this Tek ever make it to the Wiki if so what is it under?

I am receiving a couple of Kilos from Iran of Syrian rue and would like to try an extraction tek.
I was looking at the Wiki and thought to try the TAO tek. That was until this thread was thrown up with a couple of recent posts.
Was it ever confirmed if this was a better/different final product using this method?

Thank you

Kerberos

Cheers, so just a basic salt saturated solution put in the fridge to precipitate?
What pH? Is 11 ok?

No, either you precipitate the base by raising the pH (11 or so is fine yeah), or you precipitate harmala in HCl form by adding salt to an acidified solution.

For quantities and more specific info, check the harmala extraction and separation guide or some other harmala xtraction tek in the wiki.

Ok thanks.

Thought I’d post my attempt at Whiterasta’s tek, as the original is a bit light on details…

In summary, I performed this just after doing a standard Manske, with the aim of comparing yields. I did this tek in slow-time, leaving days between steps, because I had other stuff to do too ;-)

1. Powdered 100g Syrian rue seeds, and mixed with 200 ml Ethanol (95%) with ~0.5 tsp citric acid. Capped jar and let stand for 4 days. Reddish-brown liquid with turquoise sheen in daylight.
2. Strained using an AeroPress with metal disk, and washed solids with 40% ethanol (vodka) to bring total volume of liquid to 330 ml.
3. Ran this thru paper filter twice, which stained very red. Liquid lighter in colour but would probably need 20 attempts to clean completely…didn’t bother with further attempts.
4. Simmered for a few minutes, watching carefully, until alcohol smell disappeared completely. Volume now ~80ml. Added 150ml distilled water to loosen up.
5. Filtered this 5x through cotton wool (also in AeroPress) but still wasn’t crystal clear.
6. Chilled overnight to see if any sediment fell out, but it didn’t.
7. Based with ~25ml janitorial ammonia, to give pH 11. Instant precipitation. Here I tried an experiment: I poured this into a sep funnel I have, and stood it up in the fridge, and left it for about a week. I wanted to see if I could run off the sediment from beneath the liquid: it sorta worked, but the liquid just formed a kind of bore-hole through the sediment, so I got a first rush of sediment, followed by clear liquid, as the rest stayed caked inside the funnel. So, transferred everything to beaker, and let settle again.
8. Another attempt to catch the sediment: placed beaker in freezer on top of pre-cooled metal block for ~30 mins. This worked better, and the bottom of the beaker was frozen solid, so I could pour off liquid and ice-crystals from the top, before adding fresh water, to wash. Washed/froze 3x.
9. After the final washing, I didn’t add any extra water, just ~0.25 tsp citric acid to the wet harmala mix (~50ml) to redissolve harmalas as bright red citrate. Chilled overnight and a little black sediment fell out, which was discarded.
10. Mixed with 0.5 tsp CaOH. Nothing much happened, until I started to heat in water-bath, when precipitates started to form. Heated to about 60C, and pH showed 6-7.
11. Chilled overnight, and re-checked pH, which was now 8, oops! Added a pinch of citric to get pH back to 6-7, before filtering. Quite a bit of tan-coloured sediment. Filtered solution now a clear, bright red.
12. Dried in low oven (85C) for about an hour, yielding 1.3g rust-coloured harmalas citrate. With the earlier Manske extraction, I got about 3.3g freebase, but that was not perfectly pale, so probably not 100% pure.

Conclusion: I think I’ll persevere with Whiterasta’s tek. It’s a lot less messy, and you don’t have big volumes of water and sludge to deal with, which means I should be able to start with a larger amount of seeds. More finesse needed for steps 8 thru 11.