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Offlinehoodoo
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Registered: 01/28/02
Posts: 4
Last seen: 15 years, 6 months
alkoloid extraction
    #535099 - 01/29/02 05:40 PM (15 years, 6 months ago)

hey...I was just wondering if anyone here has done any alkoloid extractions...I am looking for someone who has direct experience with making this type of extraction...

thankx...


scott


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Offlinegnrm23
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Registered: 08/30/99
Posts: 6,481
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Re: alkoloid extraction [Re: hoodoo]
    #535655 - 01/30/02 08:25 AM (15 years, 6 months ago)

i have never extracted alkoloids...
i have teased some alkaloids out of plant material occasionally...
what kinda alkaloids we talkin' here?


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OfflineRedheaded1
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Registered: 01/22/02
Posts: 34
Loc: Everywhere
Last seen: 14 years, 9 months
Re: alkoloid extraction [Re: hoodoo]
    #535951 - 01/30/02 03:19 PM (15 years, 6 months ago)

I have never tried the following recipe. It is taken out of PiHKAL by Alex Shulgin. It is just a little out of my league.

SYNTHESIS: A solution of 20 g 3,4,5-trimethoxybenzaldehyde, 40 mL nitromethane, and 20 mL cyclohexylamine in 200 mL of acetic acid was heated on the steam bath for 1 h. The reaction mixture was then diluted slowly and with good stirring, with 400 mL H2O, which allowed the formation of a heavy yellow crystalline mass. This was removed by filtration, washed with H2O, and sucked as dry as possible. Recrystallization from boiling MeOH (15 mL/g) yielded, after filtration and air drying, beta-nitro-3,4,5-trimethoxystyrene as bright yellow crystals weighing 18.5 g. An alternate synthesis was effective, using an excess of nitromethane as solvent as well as reagent, if the amount of ammonium acetate catalysis was kept small. A solution of 20 g 3,4,5-trimethoxybenzaldehyde in 40 mL nitromethane containing 1 g anhydrous ammonium acetate was heated on the steam bath for 4 h. The solvent was stripped under vacuum and the residual yellow oil was dissolved in two volumes of hot MeOH, decanted from some insolubles, and allowed to cool. The crystals formed are removed by filtration, washed with MeOH and air dried yielding 14.2 g. of bright yellow crystals of beta-nitro-3,4,5-trimethoxystyrene. The use of these proportions but with 3.5 g ammonium acetate gave extensive side-reaction products even when worked up after only 1.5 h heating. The yield of nitrostyrene was, in this latter case, unsatisfactory.

To a gently refluxing suspension of 2 g LAH in 200 mL Et2O, there was added 2.4 g beta-nitro-3,4,5-trimethoxystyrene as a saturated Et2O solution by use of a Soxhlet extraction condenser modified to allow the continuous return of condensed solvent through the thimble. After the addition was complete, the refluxing conditions were maintained for another 48 h. After cooling the reaction mixture, a total of 150 mL of 1.5 N H2SO4 was cautiously added, destroying the excess hydride and untimately providing two clear phases. These were separated, and the aqueous phase was washed once with 50 mL Et2O. There was then added 50 g potassium sodium tartrate, followed by sufficient NaOH to bring the pH >9. This was then extracted with 3x75 mL CH2Cl2, and the solvent from the pooled extracts was removed under vacuum. The residue was distilled at 120-130 ?C at 0.3 mm/Hg giving a white oil that was dissolved in 10 mL IPA and neutralized with concentrated HCl. The white crystals that formed were diluted with 25 mL Et2O, removed by filtration, and air dried to provide 2.1 g 3,4,5-trimethoxyphenethylamine hydrochloride (M) as glistening white crystals. The sulfate salt formed spectacular crystals from water, but had a broad and uncharacteristic mp. An alternate synthesis can employ 3,4,5-trimethoxyphenylacetonitrile, as described under beta-D.

DOSAGE: 200-400 mg (as the sulfate salt), 178-356 mg (as the hydrochloride salt) [Erowid Note: The original text read "178-256" but this was an error. The error was found by Bo and verified with Shulgin. See the Erowid Mescaline Dosage page for a more complete discussion of the forms of mescaline].



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Offlinegnrm23
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Registered: 08/30/99
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Re: alkoloid extraction [Re: hoodoo]
    #535989 - 01/30/02 03:54 PM (15 years, 6 months ago)

well, extraction from plantstuffs...
dmt from mimosa
mesc from cactus
psiloc(yb)in from mushrooms
muscimol from the other mushrooms
harmine/harmaline from syrian rue or caapi
lysergic acid amides from mgs or hbwr
morphine from poppies
ephedrine from ma huang
caffeine from coffe or tea
(a lot of this stuff can be found at rhodium's chemistry site, as well as info at lycaeum, erowid, theforbiddenfruit, spiritplants, dmtworld, the hive, entheogen.com, ayahuasca.com, and probably several other sites as well (not to mention your university library, yaddayadda...)
so what particular plant are we looking at here anyways, huh? and how pure must the final product be? goo? colored crystals? white crystals?
usw...


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not old enough to care


Edited by gnrm23 (01/30/02 03:58 PM)


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OfflineMarleyBob
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Registered: 05/27/99
Posts: 949
Loc: USSA
Last seen: 15 years, 3 months
Re: alkoloid extraction [Re: Redheaded1]
    #536275 - 01/30/02 09:07 PM (15 years, 6 months ago)

"To a gently refluxing suspension of 2 g LAH in 200 mL Et2O, there was added 2.4 g beta-nitro-3,4,5-trimethoxystyrene as a saturated....."

LAH eh.....

Good luck with that one.


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Offlinegnrm23
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Registered: 08/30/99
Posts: 6,481
Loc: n. e. OH, USSA
Last seen: 19 days, 12 hours
Re: alkoloid extraction [Re: MarleyBob]
    #536339 - 01/30/02 10:30 PM (15 years, 6 months ago)

always looking for alternative nitrostyrene reduction...
but i fear w drift towards synthesis rather than extraction...
extractions.... temperature, solvents, pH, backwashes, sep funnel, soxhlleting....'
and then there are a few interesting plants that do their magic without alkalloids --- cannabis, kava, salvia, wormwood, just to name a few...


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old enough to know better
not old enough to care


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