GhostAliensFromMars
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Sassafras oil long term storage
I have acquired approx. 5 ml of sassafras oil via steam distillation of sassafras roots. I am storing the oil in a 25ml amber glass bottle with an
airtight plastic cap for almost a month, shown in the picture. The layer on top is water
Does anyone know if water can react and decompose safrole after a while? Should I continue storing it like this or dry it? What would be the best and
easiest way to store sassafras oil to prevent safrole decomp? I am not going to need to use this for the next year perhaps.
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Precipitates
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It will probably be okay, as strongly acidic or basic conditions are required for its hydrolysis, but if you would like to dry it:
"The oil is dried by mixing it with a small amount of anhydrous calcium chloride. After filtering-off the calcium chloride, the oil is vacuum
distilled at 100 °C under a vacuum of 11 mmHg (1.5 kPa) or frozen to crystallize the safrole out. This technique works with other oils in which
safrole is present as well."
Safrole wiki page
It can then be stored as a solid in the freezer.
Although such precautions against decomposition are probably not necessary.
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Mateo_swe
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For anyone not living in north america where the sassafrass tree grows there is another viable plant source.
Piper auritum also called Hoja Santa
https://www.kraeuter-und-duftpflanzen.de/pflanzen-saatgut/pa...
This is a climbing vine like plant with very large leaves that reeks of sassafrass smell, especially when they drop from the plant and start dry up.
Its also not a endangered plant (like the sassafrass tree) and grows like a weed in some warmer places like southern mexico from where it originates.
The large leaves has also been used in cooking and as a editable "dinner plate" where food is placed.
The leaves can be steam distilled and over 90% of the oil is safrole.
But you need quite a lot of leaves if you want a decent amount of safrole.
I have tried it and it works but as i said it takes quite a bit of leaves.
The plant grows very good inside as a house plant if you dont mind having a jungle inside.
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GhostAliensFromMars
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If I wanted to make safrole in larger quantities (not for MDMA of course), would it be easier and more cost effective just to synthesize it from
eugenol ?
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Mateo_swe
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Yes.
Extracting it from any natural source is way more work and hassle than a syntetical route.
Maybee if you had a big rootsystem from a whole sassafrass tree and have access to big steamdistillers it could be a viable route.
You could start from Eugenol, Vanillin, catechol or helional, there are plenty of options.
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GhostAliensFromMars
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What would be the easiest method if I were to start from eugenol?
Thanks
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Mateo_swe
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I would try the route in the attached paper and then methylenate the product to form the methylenedioxy ring and you will have your safrole.
But i havent tried it myself so i dont know how well it will do i real life/amateur lab.
The second methylenation step have been done by some members in this forum but on a slightly different substrate.
Se this for example
https://www.sciencemadness.org/whisper/viewthread.php?tid=28...
Just rename file to xxx.pdf, it wont show the correct name on the pdf file.
Attachment: phpYS9GMb (430kB)
This file has been downloaded 129 times
[Edited on 2024-11-18 by Mateo_swe]
[Edited on 2024-11-18 by Mateo_swe]
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GhostAliensFromMars
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Thanks for the resources, correct me if im wrong but is this process: (https://www.youtube.com/watch?v=c-BAXOgC0YU) the same as the one in the file?
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Mateo_swe
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No, it is not the same process, he used another older process.
The one in the attached paper uses AlI3 (formed in situ from iodine and aluminium) and hopefully gives a better yield.
But one never know until one tried it.
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GhostAliensFromMars
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Would you know if using toluene instead of acrylonitrile as the solvent will work? Acrylonitrile is unfortunately unavailable to me.
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Mateo_swe
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Why dont you talk with some of the sellers in the "Reagents and Apparatus Acquisition" section of this forum.
They can help you get some MeCN (Acetonitrile).
Depending on your location one of the sellers can probably help you.
I have had good purchases from chemship1978 in the past, so if you are in Europe it´s an option.
I dont know if you can substitute the MeCN for some other solvent, maybe someone else knows this?
The MeCN isnt involved in the mecanism that makes this work though, something that might suggest that other solvents are mabye usable.
If i had to try something i would guess DMF or cyclohexane might work.
They are mentioned in the paper.
I am not good enough in chemistry to know if the above suggestions are good or even a dangerous combination.
You should get a second opinion on these solvents.
If in Europe, https://www.laboratoriumdiscounter.nl/en/acetonitrile-999-ex...
[Edited on 2024-11-29 by Mateo_swe]
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zed
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UMMM. Without a license, access to this reagent is relatively difficult.
If you reside in the warm Southern USA; Safrole can be salvaged from older Camphor Trees. The wood is very rich in Safrole.
First, the wood should be chipped. Then, the chips are subjected to steam distillation. Camphor will crystalize out of the oily distillate.
Thereafter, the oil that remains is very rich in Safrole; which may be isolated by fractional distillation.
The bonus being that a mature Camphor tree is quite large, and non-native to the USA. The relevant property owners, might actually pay to have the
tree removed.
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GhostAliensFromMars
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could I just instead perform a solvent extract of the camphor wood with ethanol, and fractionally distill out the safrole?
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Mateo_swe
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Maybe, but that depends on what other compounds are in the camphor wood and what their boiling points are.
Especially if there are any other compounds with similar boiling points as the safrole.
Steam distillation has been known to work for safrole type compounds.
If you try steam distillation, make a external steam generator and feed the steam into the bottom of the vessel with the camphor chips using a hose.
This is more efficient than just put the chips in water and let it boil.
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GhostAliensFromMars
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just tried this today, here's my results.
In my front yard is a relatively large camphor tree. I used a hammer and chisel to carve off 100g of the sapwood near the roots of the tree, the chips
where blended and placed in a 1 litre RBF. Since I don't have a soxhlet on hand, I opted to reflux it. 300ml of 95% ethanol, distilled from methylated
spirit, was added and it was reflux for 5 hours.
The EtOH was filtered and the maroon liquid was heated to distil off the ethanol. Near the end after close to 250mls of etoh had been removed, solid
brown particles appeared in the boiling flask. Assuming these were just taninns /pigments, I filtered them out. A small amount of the filtrate was
reacted with conc h2so4 and the results where very similar to "shikimol's" reaction with conc h2so4, producing a dark purple ppt and a sweet fruity
odor. I plan to repeat this experiment on a much larger scale, kilograms of camphorwood and will attempt to fractionally distill out the "shikimol" to
separate it from the camphor. Will post again with pics soon.
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Mateo_swe
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Thats intresting, nicely done.
Please keep us updated on your progress.
I read somewhere that champhor trees come in a few different varietys and one of those has a high concentration of safrole.
But maybe all camphor trees has a bit at least.
Unfortunatley no camphor trees can live in my climate, at least i dont think so.
I wouldn´t be suprised if some other tree variant contain similar compounds and can live in a bit colder climates.
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GhostAliensFromMars
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Do you know of any other ways an amatuer could detect the prescene of the allylbenzene? I set up for fractional distillation and removed all the
ethanol. I then applied a strong vacuum of 10-20mmhg and the temperature stayed at 112c for a few hours. There was a VERY strong camphor odor in this
fraction with a faint sassafras odor, so I am assuming this was the camphor/linalool/cineole/terpine fraction. The liquid in the boiling flask turned
to a thick black viscous oil before I reach the expected BP of the allylbenzene, which was at 148c. I collected about 4mls of this fraction, it was
brown and it did have a slight camphor smell but the smell of sassafras was VERY distinct. I'm guessing it was at least 50% safrole mixed with
camphor. A second fractional distillation of this should be effective.
do you know any other methods to identify the concentration of safrole in oils that don't require high tech expensive equipment? I also thought about
freezing the ethanol mixture and il try this next run. I've been refering to the pdf below for identification methods. I have orderd a sample of
camphor oil online, probably don't contain the allylbenzene but I would like to compare this oil with my extracts from the tree and see how it reacts
with conc h2so4
Overall i am pleased with these results. 4ml of 50%-ish safrole from 620g of fresh camphor sapwood is great and will be scaled up. I am still
considering building a large steam distiller as working with litres of flammable solvents is a pain in the ass.
https://www.unodc.org/documents/scientific/SCITEC21_07fin.pd...
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