Author Topic: (MhRB) - EtOAc as extr. solvent  (Read 5294 times)

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kurupira

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(MhRB) - EtOAc as extr. solvent
« on: July 22, 2002, 11:18:00 PM »
swik is curious about using ethyl acetate as a extraction solvent on mhrb dmt extraction. All papers swik had seen on dmt synthesis uses it on final extraction (so high affinity), but  never got any paper on mhrb extraction which it's used.  So has anyone ever been experienced using this sovent?
here it's cheaper and more otc than dcm(which is the best swik have dreamed with).

Ps. swik has at hands a paper showing an extraction which is a direct partition of the ground plant material w/ cholroform/NH4OH (pH ~9), and workup of the cloroform extracts as usual. The author said it was to avoid tannins and saponnins which are extracted w/ methanol, the yields are 1% from the dried root bark(fucxxxx good! 8) ) swik never deamed bout'it, but will...

Ghost_Of_BT

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Could you post that chloroform/NH4OH extraction ...
« Reply #1 on: July 23, 2002, 06:33:00 AM »
Could you post that chloroform/NH4OH extraction method in detail?

ClearLight

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Bufotenine which should work for dmt...
« Reply #2 on: July 23, 2002, 09:57:00 AM »
Johnathan Ott's extraction procedure:

( it appears that EtOAC will crash out the tryptamines, but I do not know if this has been verified )


ISOLATION AND PURIFICATION OF BUFOTENINE FREE-BASE

Coarse-ground powder of 125g of seeds of A. colubrina var. Cebil was stirred twice for eight hours in 500 ml of 96% ethanol 1% tartaric acid, the combined filtrates concentrated to 150 ml and diluted with 200 ml water in a separatory-funnel, causing precipitation of considerable fat. The pH was adjusted to 3-4 with concentrated hydrochloric acid, and the solution defatted by shaking six times with chloroform, which was set aside. The defatted extract was basified to pH 8-9 with ammonium hydroxide, then again extracted eight times with 200 ml chloroform; the combined chloroform extracts were concentrated to a foamy, yellowish oil that dissolved completely in 50 ml hot ethyl acetate, then concentrated to 15 ml and refrigerated overnight. In the morning there were a brace of minuscule rosettes of dark-brownish crystals growing at the base of the flask, which was alternated between periods under refrigeration and standing unstoppered at room temperature during 48 hours, leading to the formation of large masses (some greater than 1cm) of dark-brownish, prismatic crystals. The mother-liquor was decanted and the crystalline mass rinsed with cold ethyl acetate dried over magnesium sulfate, then dried under reduced pressure to yield 4.1 g of large, free-flowing, sparkling brownish crystals. These were twice recrystallized from dry ethyl acetate, yielding 3.87 g of off-white bufotenine free-base crystals (3. 10%), m.p. 125-126' C. Despite loss of chromophores on recrystallizations, the melting point remained 124-126'.


Infinite Radiant Light - THKRA

kurupira

  • Guest
New method to bee tested...
« Reply #3 on: July 24, 2002, 12:24:00 AM »
It's a brazilian paper
here it goes...
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(AN. FAC. MED. UNIV. RECIFE, V 21, ns 1-2, p. 9-33, JUN-DEC 1961)
ANTÔNIO CESÁRODE MELO
JACYREMA ALVES BANDEIRA
...
(A) CHEMICAL PART

We worked w/ roots of 'Jurema preta', from Arcoverde city, i.e. same origin of roots used by Prof. Gonçalves de Lima, meaning the same botanic classification as Mimosa hostilis Benth.

-New method to isolate Nigerin (Dmt)-

Due to the abundance of tannins on the MhRB, we tried a tech to isolate the alkaloyd, avoiding interference of the said component on our work. We got good yields w/ the following tech:
 The air dried root bark was ground (how much?) , and treated under mechanical agitation w/ chloroform in presence of a diluted solution of NH4OH, the upper layer showing pH 9.0. After filtration the solid matter was again extracted until it shows a weak response to Wagner reactive. (I2 + KI). The chloroform extracts were reduced under rotovap until a syrup residue. This was treated several times w/ small portions of H2SO4 1N. The insoluble fraction was discarted. To the yellowish acid solution there was added chloroform and the pH was raised to 9.0 w/ diluted NH4OH solution the chloroform layer was separated and this was repeated several times, the chloroform extracts were washed w/ water, until the water layer shows pH near 7. The chloroform layer was dried w/ Na2SO4, filtered and reduced under rotovap. The syrup residue was left 24h on a dessicator (NaOH pellets or conc. H2SO4), and crystslised as small yellowish concentric needles, m.p 40.0-43.0oC. W/ this tech we got an 1.1% yield of crude alkaloyd content from the dried root bark.
Due to the colour of the crystals and the hygroscopic caracter, we tried a purification. We treated them in diluted H2SO4 solution (pH 2.0)under agitation w/ Merck activated charcoal (Methylenblautiter 10-11), after filtration we followed the procedure described above, and we got a 0.98% yield of a less hygroscopic whitish-yellowish crystals w/ m.p. 42.0-44.0oC.
...
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good job, no? ;)

ClearLight: The Ott's procedure uses chloroform as the first extraction solvent of the alkaline plant extract, but thanks anyway...