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Manske Extraction w/Freebase Conversion


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#1 Phineas_Carmichael

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Posted 25 June 2010 - 04:15 PM

My buddy Freddy has been messing around with his chemistry set and a big old bag of Syrian Rue seeds. Here's some pics! :)

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100g seeds were boiled 3 times for 30 minutes each in a solution of ~5% Acetic Acid (Distilled white vinegar right out of the jug is usually 5%)

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The seeds were strained through a wire strainer and collected in 1 quart jar. Freddy ended up with 700mL of Rue tea. A wise chemist would have waited overnight and decanted off the solids but Freddy, knowing he was going to convert to freebase, just straight away added 70g of non-iodized sea salt with no anti-caking agents to the still warm tea and stuck it in the fridge overnight.

 

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12 hours later he siphoned the tea off the crystals stuck to the jar,

 

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Filtered, dried, and weighed the crystals for a yield of 4.688g or ~4.7% acetate salts.

 

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This was dissolved in 200mL of ~5% acetic acid solution and filtered

 

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Baking soda was added dry to this solution until it stopped fizzing when added. The solution was still quite red at this point.

 

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A saturated sodium carbonate solution was created and added to the neutralized tea until adding more solution did not change the color.

Freebases are dropping out in the fridge right now, will update later.

EDIT: It's later, here's the freebases so far...
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Edited by Sidestreet, 10 September 2016 - 04:18 PM.
Update

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#2 Phineas_Carmichael

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Posted 26 June 2010 - 12:30 AM

~2.5g freebase harmala alkaloids

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#3 shiitakegrower

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Posted 26 June 2010 - 01:33 AM

Wow, any idea how long its stable in that form?

#4 Raoul Duke

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Posted 26 June 2010 - 04:43 AM

How many Mg's per dose?

#5 Phineas_Carmichael

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Posted 26 June 2010 - 10:39 AM

Wow, any idea how long its stable in that form?

I have no idea, its stored under CO2 in a test tube, with the test tube sealed in a vacuum bag so, darn near forever as far as I'm concerned.

How many Mg's per dose?

Syrian Rue contains 2-7% alkaloids, according to Ott's surveys. A sufficient dose of P. Harmala seeds for Pharmahuasca is said to be 3-5 grams. Assuming a *perfect* extraction[not likely outside a lab] this would yield 135-225mg B-Carbolides at 4.5% alkaloid content.

Assuming a 2% content: 3-5g P. Harmala=60-100mg extract.

Assuming a 7% content: 3-5g P. Harmala=210-350mg extract.

[Both these assume 100% yield, probably difficult with home chemistry]


Instead of choking down 3 grams of seeds or ounces of nasty tea, a 200mg pile of brown powder can be dissolved easily into orange juice or even smoked.

Edited by Phineas_Carmichael, 26 June 2010 - 03:46 PM.


#6 McDozd

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Posted 26 June 2010 - 10:45 AM

Nicely done Phin!
MD
:bow:

#7 waylitjim

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Posted 26 June 2010 - 10:47 AM

Very cool Phineas, love to see what you'd do with MHRB.

edit...just found your thread A/B vs STB Side By Side

#8 kcmoxtractor

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Posted 26 June 2010 - 10:49 AM

Nice one buddy, archive material after the thread slows!

#9 Phineas_Carmichael

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Posted 26 June 2010 - 11:47 AM

Very cool Phineas, love to see what you'd do with MHRB.

edit...just found your thread A/B vs STB Side By Side


That reminds me, I should update it...

http://mycotopia.net...=1&d=1312960278

Thanks for the compliments everybody. Clandestine Chemistry FTW! ;)

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Edited by Phineas_Carmichael, 10 August 2011 - 02:13 AM.
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#10 Disumba

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Posted 26 June 2010 - 02:39 PM

Okay, now I would like to see a total alkaloid extraction of B. caapi.. :p The THH, harmine and harmaline.. I hear the THH is one of the more difficult ones..

#11 Raoul Duke

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Posted 26 June 2010 - 04:16 PM

That reminds me, I should update it...

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Thanks for the compliments everybody. Clandestine Chemistry FTW! ;)


Whats the nice white fluff in the middle? Pure D?
The goo vile on the right looks scary!
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#12 Phineas_Carmichael

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Posted 26 June 2010 - 04:45 PM

Whats the nice white fluff in the middle? Pure D?

Pure as the driven snow. :thumbup:

The goo vile on the right looks scary!

Scares the stuffing out of me, that's for sure! :lol:

#13 BioTron

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Posted 26 June 2010 - 10:12 PM

Try taking the acid extract and basifying to drop the freebase form, then decant and filter and you'll end up with a freebase without creating the salt first. i'll get some pics up and show you all.

#14 BioTron

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Posted 26 June 2010 - 10:14 PM

i just noticed your comment about smoking. The dosage for smoking is much less than oral, somewhere around 35-50mg should be sufficient of the freebase.
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#15 Shadowlord

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Posted 27 June 2010 - 01:19 AM

Very Nice Phineas.
Well Done.
I plan to do some Rue extracting soon and your thread will come in handy.

#16 Ferretious

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Posted 27 June 2010 - 03:15 AM

I have 100gms of syrian rue seeds..........Hmmmmm:eusa_thin

#17 BioTron

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Posted 27 June 2010 - 12:44 PM

I suggest playing with the rue extraction before doing an MHRB extract, it is much easier, being there is no need to use a sep funnel.

Phin, if you have some more seed lying around try this:
Extract seeds with boiling methanol by decanting
Add vinegar to the methanol soaked seeds extract and decant
Extraxt with methanol again
Extract with vinegar
Extract with water
Combine all extracts and ditch the seeds

Wash aqueous extract with naptha x3

Basify to drop freebase harmalan alkaloids
At this point the alkaloids are brownish

I redissolved in minimal ammount of vinegar, basified and collected the crystals that form. Doing this 1x produced a light tan crystal that didnt get much cleaner repeating the process, and a naptha wash of the acidified extract didn't really discolor so i believe the nonpolars are pretty much cleaned from the harmalan extract.

#18 translucentwaves88

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Posted 27 June 2010 - 01:37 PM

So swim just got done straining syrian rue and was wondering if epsom salt would work instead of sea salt. Cause that is all that swim has laying around the house. Plus swim knows that epsom salt is usually used in MHRB extractions. Swim decided to use the epsom salt and will see if it works out. Will keep you updated...

#19 Phineas_Carmichael

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Posted 28 June 2010 - 03:23 AM

Phin, if you have some more seed lying around try this:
Extract seeds with boiling methanol by decanting
Add vinegar to the methanol soaked seeds extract and decant
Extraxt with methanol again
Extract with vinegar
Extract with water
Combine all extracts and ditch the seeds

Wash aqueous extract with naptha x3

Basify to drop freebase harmalan alkaloids
At this point the alkaloids are brownish

I redissolved in minimal ammount of vinegar, basified and collected the crystals that form. Doing this 1x produced a light tan crystal that didnt get much cleaner repeating the process, and a naptha wash of the acidified extract didn't really discolor so i believe the nonpolars are pretty much cleaned from the harmalan extract.


:amazed: Interesting... a defat step... Freddy, being the purity freak that he is, will be pleased to have something new to tinker with. Thanks!

So swim just got done straining syrian rue and was wondering if epsom salt would work instead of sea salt. Cause that is all that swim has laying around the house. Plus swim knows that epsom salt is usually used in MHRB extractions. Swim decided to use the epsom salt and will see if it works out. Will keep you updated...

Let us know what happens, but I don't expect any magic. I've been proven wrong before, though...

Epsom salts absorb water so are used to remove traces of water from non-polar solutions in MHRB extractions. The table salt (doesn't have to be "sea salt" but avoid iodized salt and anti-caking agents if you can) in the Manske extraction is to force the harmala salts out of solution. Harmala salts are soluble in pure water, but not in salt water.

Edited by Phineas_Carmichael, 28 June 2010 - 03:37 AM.


#20 translucentwaves88

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Posted 28 June 2010 - 05:44 PM

Epsoms salt did work out and made a fine brownish powder as pictured on the left...So it worked and was amazed that it did...:)
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