So I had a concentrated acid solution of Ephedra plant kept for a long time. It had a blurry brown color with a strong smell. Yesterday I decided to extract some alkaloids from it and added NaOH solution to turn salts in freebase. After raising pH, brown precipitate formed immediately after which I waited overnight for solution to settle. This morning, I removed excess fluid and added some diluted HCl acid to turn freebase back to acid. After adding, solution became clear and white fluffy stuff precipitated and settled on the bottom. As I know both ephedrine and pseudoephedrine chloride salts are soluble in water, so it was unusual to see some precipitate in the acidic solution. Any ideas? I did not use DI water, just tap water which have some minerals but I don't think there would form some insoluble chlorides there. PS: the solution was not really dilute (there was not too much water present) so I think after adding HCl, alkaloid salts dissolved in water and created a saturated solution, and the remaining salts just precipitated out. I'm gonna filter the white fluff and dissolve in some diluted HCl acid to see if this was the case.
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N&PD Moderators: Skorpio | thegreenhand
Ephedra acid-base extraction gone weird?
- Thread starter dzaocom
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Limpet_Chicken
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You could try steam distillation of the base. Or basifying, keeping it as a paste and then using liquid butane to extract it.
Limpet_Chicken
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Yes your going to need organic solvents, Methanol would give a (very, very) crude extract and allow for filtration of the plant patter. A Soxhlet wouldn't be a bad thing either.
A handy selection of solvents for the purification would be methanol, acetone, diethyl ether, benzene or toluene (benzene has a lower boiling point and is similar in solvent properties to toluene but tolly is MUCH safer, because benzene is pretty carcinogenic and has a propensity towards causing leukaemia) Toluene however, despite the similar structure, is, due to the methyl group (its methylbenzene) not flat, planar in structure like benzene is and as such cannot slip in and intercalate DNA. Generally benzene should bee avoided unless you are capable of handling it safely (I.e make sure your gas mask is rated for organic gases and vapors and that the cartridges are fresh, do not use or prepare it indoors (it can be made if it cannot be bought, by destructive dry distillation of calcium benzoate, the distillate being benzene) if you have not got a fume hood, the alternative is to do it outside, ideally when the wind is blowing in a direction that does not carry the fumes back to you. Wear protective equipment at all times when using it, its nasty ass stuff. My old chem teacher in school knew somebody that died from leukaemia, most likely (this was back in the day when such things were considered normal practice) due to mouth-pipetting benzene.
A handy selection of solvents for the purification would be methanol, acetone, diethyl ether, benzene or toluene (benzene has a lower boiling point and is similar in solvent properties to toluene but tolly is MUCH safer, because benzene is pretty carcinogenic and has a propensity towards causing leukaemia) Toluene however, despite the similar structure, is, due to the methyl group (its methylbenzene) not flat, planar in structure like benzene is and as such cannot slip in and intercalate DNA. Generally benzene should bee avoided unless you are capable of handling it safely (I.e make sure your gas mask is rated for organic gases and vapors and that the cartridges are fresh, do not use or prepare it indoors (it can be made if it cannot be bought, by destructive dry distillation of calcium benzoate, the distillate being benzene) if you have not got a fume hood, the alternative is to do it outside, ideally when the wind is blowing in a direction that does not carry the fumes back to you. Wear protective equipment at all times when using it, its nasty ass stuff. My old chem teacher in school knew somebody that died from leukaemia, most likely (this was back in the day when such things were considered normal practice) due to mouth-pipetting benzene.
Overexposure to benzene will knock you out and not in a good way in a dangerous way like your working doing your job be in manual labor painting where its in paints and stuff ect or chemistry as a solvent exposure even briefly is likely toxic to the motor neurons causing tremor and long term dysfunction of the cerrebellum, cognitive dysfunction, rage, total amnesia, fainting, sudden cardiac death, and coma.
Please becareful if using these for whatever reason
Please becareful if using these for whatever reason
Limpet_Chicken
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Pyrolytic distillation of Ca benzoate? Bet the lead salt might work too.
Isn't petrol in the EU (UK rather) these days meant to be low in benzene? or is there actually enough in there for it to be worth fractionating? More out of curiosity than need really, since I'd buy it if I needed it in sufficient purity to be a reactant, rather than muck about fractionally distilling petrol.
Isn't petrol in the EU (UK rather) these days meant to be low in benzene? or is there actually enough in there for it to be worth fractionating? More out of curiosity than need really, since I'd buy it if I needed it in sufficient purity to be a reactant, rather than muck about fractionally distilling petrol.