Best way to isolate safrole from sassafras essential oil

BrownRiceSyrup

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Sooo i finally got some sassafras oil and im seeing several ways to do this...

The most common seem to be:
the freeze crystalization of safrole
vacuum distillation
liquid/liquid extraction

( https://www.drugtimes.org/ecstasy-3/safrole.html kind of goes over a bunch of methods if anyones curious. written by strike eons ago)

What ways have worked for you guys? any tips? thoughts?

Ive got the vacuum distillation setup and everything needed to go just about any route with it... Hoping to hear other peoples thoughts and experiences before i commit to a method though...
 

Loki12

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Vesp topic:
"cant get safrole? FREEZE IT!"

Go to page 2 and start reading from there, I believe you should find most of what you need by just going over that second page from top to bottom. Let me know if it works out for you or not!
 

Osmosis Vanderwaal

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Seems like freezing it would be a great start, followed by vacuum distillation to achieve reagent grade, which is never a terrible thing but may be unnecessary, depending on what you plan to do next
 

G.Patton

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It is the best way, I think. Hi.
 

Loki12

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@BrownRiceSyrup
@G.Patton
I have had much success with the method I posted above actually; since posting my reply on this thread I have had time to experiment.
I was not fortunate enough to get my hands on sassafrass oil however, so I cannot comment directly on the process, however when researching procedure I found that the essential oil I chose was much harder to process and was even told to give up when asking for help. Fractional vacuum distillation yields were poor and the fractions were too close together I feel.
At the end, I divvied up the oil into 1l clear glass bottles and stuck it in an apartment freezer, I believe at first nothing happened as the small fridge barely had anything in it, so I believe the temperature was not low enough. I did not have a seed crystal either.
After about 2 weeks, white precipitate formed out of the oil which was observed clumped and floating, additionally, small crystals formed on one of the bottles walls which was placed in the freezer in a horizontal position. The oil from the horizontal bottle was poured quickly into another container, bottle was closed in room temperature and crystals proceeded to turn into a liquid once more. The other bottles were taken out and oil was decanted very slowly to retain the sperm-like substance in the bottles. The bottles were allowed to come back to room temperature and melt the substance within (to collect all frozen parts of the white precipitate which now remained, but also was observed formed in small quantities on walls of bottles).
The very much lighter now liquid oil was combined into one smaller glass bottle and placed for another 10 or more days into the shit freezer... Oil was divvied up once again into 1l and bottles were all placed horizontally..
Imagine the surprise, when opened the freezer after this time, found more milky precipitate floating in bottles of oil and the small bottle in which the substance was combined, was almost completely solid and crystallized beautiful shapes all over the inside wall on which it was laid.

I can give only one piece of advice, which was the matter of discussion in the thread I referred you to; the substance which crystallized out for me, only did so effectively, when it was separated from the mother oil. The white milky substance which freezes out of the oils, does not stick to the bottom or the sides, maybe in higher concentrations it would, for me it simply floats and much care must be taken to decant the oil and not pour the milk with it. I have separated almost all of it and will be running more tests when there is time available, I would certainly like to freeze the oil and try separation by centrifuge, however, I just do not have the time to try and get this "small" amount of substance out and play with it, as I have customers to satisfy on a larger scale. When I get some time, I will research this further, I have some photos, I might make a thread to give back to this community.. With better equipment, I will for sure re-visit this method, as then maybe it could be worthwhile on a larger scale.
 

G.Patton

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I guess you can use long vigorous column in order to carry out this distillation more carefully in addition to the freezing procedure.
It would be great!
 

oldkaw

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You guys use a steam still to separate sassafras oil from roots?
 

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H @BrownRiceSyrup - so that link is from Strike's Total Synthesis II. An OK book in my opinion but I"m starting to have some doubts about it. I have been experimenting with my Sassafras using the 30% Acetic Acid and Ethanol method Strike mentions. Based on multiple experiments that method either doesn't work or I don't have real Sassafras. So I'm in the process of trying to find a professional lab test whether I have Sass or not. Any recommendations would be appreciated. I'm curious what your best tried and true method for isolating Safrole from Sass method is at the moment.

One thing did get right is that Illicium Parviflorum does contain Safrole in the leaves and branches. I have several "Florida Sunshine" growing in my yard presently. A few years I'll get the precious essential out of them and there will be no doubt if I have Safrole or not. In meantime though, I want to see if I have scored the best Sass hookup in the US or if this just another fucking con job.

Nothing like getting through a tedious fractional distillaton for hours, letting your PdCL stir overnight in Methanol, deal with a hydroquinone mess, vac distill for hours and come up jack diddly fucking squat
 
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