Sciencemadness Discussion Board

Real sassafras oil from roots!

chemist1243 - 19-10-2020 at 11:26

Back story:

I live in sort of a rural area with lots of forest in eastern North America. The sassafras tree is fairly rare and isn’t as abundant as maple or oak, but every once in a while there are sweet spots with many many sassafras trees clustered together. My property has one of these sweet spots centered around a small swamp, in which i counted 50 or so saplings and mature sassafras trees before i stopped counting, and there are many more than that.



I seized the opportunity and delicately extracted an entire tree using a large tractor with a bucket, giving me access to the entire root system of that tree but sadly also killing it. I cover the dirt back up and managed to preserve all the surrounding sassafras trees.

In total I was able to fill a little over a 5 gallon bucket with soft fleshy and fragrant rootbark, which was very oily. I broke up the root bark with my hands over around 2 hours to get a lot of half inch bits of rootbark, which i washed and removed all the twigs and dirt from in a strainer.

Through much trial and error, i developed an extraction method that gave good yields and didn’t require anything like passing steam through an elavated flask or using a pot still, although pot stills make this whole thing much more easy.

Procedure:

Sassafras rootbark is added to a blender along with an equal amount of tap water. The mixture is blended to get a thick dark brown slushy. This is added to 1 liter flask and set up for simple distillation using and oil bath coupled with tin foil insulation to maintain the right temperature. At a little over 96C hydrosol along with little drops of sassafras oil started coming over.

You could visibly see the oil droplets slide down the condenser, it was enchanting!

Now the hard part. See, hydrosol, or at least sassafras hydrosol, isn’t easy to separate from sassafras oil. First I tried using a seperatory funnel like The poor mans chemist, but that didn’t work because oil droplets would float on top of the hydrosol and stick to the sides of the funnel. I cant expect anyone to go out and buy a centrifuge so that was off the table too, however if you have one then use it becuase it works quite well apparently.

You must use a syringe. You simply load up hydrosol/oil into a syringe. Tilt it upside down with the spout facing upwards and let the oil settle out to the bottom. Then squirt off the upper water layer(yes, you will get a little wet) until you are left with only the oil. Perfecto, Now squirt the oil into a bottle. Do this until you have at least 30ml.

Drying:

This step is optional but preferred. The one disadvantage is that you will lose some of your oil however if you managed to get 100ml+ quantities of oil this step will be of benefit, but skip it if you don’t mind a few water droplets floating around your oil. Simply swirl around the sassafras oil with some dry magnesium sulfate and then decant the dried oil into a dry storage container.

I managed to get around 30ml out of a half a kilo of root bark, but you increase the yield when you distill the same root bark 2 or 3 more times to get it all out. Mine is slightly oxidized because its been sitting out since last fall, but it still smells woody and has the classic root-beer/licorice smell, however the woody smell is stronger than the 2 former. I have used about 1.5ml of it to get the stink of DMSO out of my lab and it worked okay, but I’m sure its got loads of other things its good for. If you smoke cigarettes then try smearing a bit on one and see if you like it, it gives something like a menthol kick but dont over do it, I’m sure the combustion products are worse or just as bad as tobacco.

I’m posting this because i know its pretty much damn near impossible to get it any other way, and this method is the least labor intensive out of the ones Ive tried. If you have a pot still then use it because you’ll be able to fit a lot more slurry in one than you would a flask.

Enjoy :D



9FA1636F-294C-4BBF-8513-486F992774C8.jpeg - 1.3MB

Cou - 19-10-2020 at 11:28

epic x)

Chemorg42 - 19-10-2020 at 12:25

Interesting, if it is this difficult to extract, how do the large illegal operations obtain it?

Corrosive Joeseph - 19-10-2020 at 12:31

They don't....



/CJ

arkoma - 19-10-2020 at 13:00

Come to the dark side..........

Sassy is endemic where I live too.

monolithic - 19-10-2020 at 13:44

Quote: Originally posted by Chemorg42  
Interesting, if it is this difficult to extract, how do the large illegal operations obtain it?

https://www.alltreatment.com/destruction-of-the-sassafras-tr...

chemist1243 - 19-10-2020 at 14:41

Quote: Originally posted by Chemorg42  
Interesting, if it is this difficult to extract, how do the large illegal operations obtain it?


Simple: hide
Apparently its done on a mass scale using a larger more safrole rich tree. They use the cover of the jungle to hide large 1000+ liter welded metal distillation apparatus to steam distill out safrole from the wood chips. here’s an interesting video on it:

https://youtu.be/lASLSC5L_yw

brubei - 19-10-2020 at 15:02

Quote: Originally posted by chemist1243  
Back story:

i bought some on internet without issue.

smell is very pleasant, powered with a strong aroma of borderline subversion.


arkoma - 19-10-2020 at 15:32

Camphora genus trees. Endangered. There are enough {i}Sassafras Albidum trees here if I decide to scratch that itch.

chemist1243 - 19-10-2020 at 15:46

Quote: Originally posted by brubei  


i bought some on internet without issue.



Have you measured the density of the oil you bought?

zed - 19-10-2020 at 19:04

Oh, I don't think it is illegal to steam distill sassafras roots.

But, I will say this. Do it fresh. Saffrol is pretty volatile. Year old bark, will have lost a lot of its oil content.

Sassafrass root bark isn't the most common source of Saffrol.

More commonly, derived from Camphor wood.

A few years back, such trees were abundant in Florida and Southern California.

Considered a pest species.

A lot easier to just buy a bottle full of the oil. But, I've been told, that isn't so simple anymore.

Mateo_swe - 20-10-2020 at 01:04

There is a more environmentally friendly source of safrole.
The plant Piper Auritum, also called Hoja Santa and the rootbeer plant is a very fast growing plant with huge leaves.
The essential oil can be collected by steam distillation and is mostly safrole.
I have a few of this plant and it really smells strongly of licorice.
The fast growing and large leaves of this plant makes it a very good alternative to destroying the rare Sassafras trees.


brubei - 20-10-2020 at 01:13

Quote: Originally posted by chemist1243  
Have you measured the density of the oil you bought?
nope

i can do TLC to compare with OP.

Mateo_swe - 20-10-2020 at 05:11

There are much sassafras oil circulating that arent the real sassafras safrole rich oil.
Since FDA has classed Safrole as an possible cancerogen its banned from all food and drinks where it was commonly used before the ban.
So many "replacements" have been made not only to scam people from the real oil but as a substitute for it in food and drinks.
Since sassafras oil is so expensive there probably are many who would sell substitutes as real sassafras oil so i would try to test any oil bought to verify it.

yobbo II - 20-10-2020 at 10:31


Purchased saffarfas oil over the counter from a chemist that ordered it for me about 30 years ago. It wassent saffaras, something else.

brubei - 20-10-2020 at 12:49

Quote: Originally posted by Mateo_swe  
There are much sassafras oil circulating that arent the real sassafras safrole rich oil.
Since FDA has classed Safrole as an possible cancerogen its banned from all food and drinks where it was commonly used before the ban.
So many "replacements" have been made not only to scam people from the real oil but as a substitute for it in food and drinks.
Since sassafras oil is so expensive there probably are many who would sell substitutes as real sassafras oil so i would try to test any oil bought to verify it.
Interesting. i would check mine with tlc and some reagent.

I think i have some handbook for plant tlc.

brubei - 20-10-2020 at 13:05

here is reference work
Plant drug analysis, 2nd (Springer)

Attachment: oil.pdf (238kB)
This file has been downloaded 45 times


chemist1243 - 20-10-2020 at 13:38

Do TLC on your oil, see what comes up. Depending on how many years ago you bought it, its likely a fake.

karlos³ - 20-10-2020 at 13:59

The hydrosol isn't worth to go after, I know that as one of ours extracted ten kilo of roots(whole roots, chipped), with the result being 240ml of safrole(forgot the amount of the natural oil, but read the report for yourself if you're interested in this.
Its called "an oldie but goodie - xxx goes from roots to crystals" in the publication section next door.

Also, I hope it wasn't mum's blender you used for shredding the plant material :D
You are planning on doing what with the oil? isolating the main compound is obviously one of the ideas driving your motivation for this project ;)

I would be interested how much of the oil turns out to be your desired compound.
As the 240ml above, of twenty times as much material, were after vacuum fractionation and the desired substances even already distilled twice in vacuo, and thats all what he got out.
So thats just eight times your products volume, made from twenty times of what your substrate weighed.
Although yours sounds like it was superior bark mostly and not whole chipped roots.

Besides this, nice and interesting piece of work.
You really should take a look into the mentioned thread, and all the other pieces of work from the same person(actually his neighbor), they all start with the isolation of ethereal oils and how to process each of them to the respective final product.

arkoma - 20-10-2020 at 16:01

Here in the Central United States, sassafras is anything but rare/endangered. They grow like weeds. True Sassafras Albidium

*edit* SOUTH Central US

[Edited on 10-21-2020 by arkoma]

Amos - 20-10-2020 at 17:42

Anywhere fairly-well drained and especially at the edge of a forest and in clearings is fair game for them in Kentucky. The little clonal groups they tend to form are especially easy to see this this time of year, bright scarlet or rust-colored foliage. I never miss the opportunity to tear off a leaf passing by, they have their own delicious smell!

draculic acid69 - 20-10-2020 at 17:44

Quote: Originally posted by Chemorg42  
Interesting, if it is this difficult to extract, how do the large illegal operations obtain it?

One documentary showed ppl in Asia cutting carfulls of sometrees roots
out illegally which then gets processed and sent to Vancouver Canada.
Apparently tonnes of oil get sent there from Asia

chemist1243 - 20-10-2020 at 18:02

Quote: Originally posted by karlos³  
The hydrosol isn't worth to go after, I know that as one of ours extracted ten kilo of roots(whole roots, chipped), with the result being 240ml of safrole(forgot the amount of the natural oil, but read the report for yourself if you're interested in this.
Its called "an oldie but goodie - xxx goes from roots to crystals" in the publication section next door.

Also, I hope it wasn't mum's blender you used for shredding the plant material :D
You are planning on doing what with the oil? isolating the main compound is obviously one of the ideas driving your motivation for this project ;)

I would be interested how much of the oil turns out to be your desired compound.
As the 240ml above, of twenty times as much material, were after vacuum fractionation and the desired substances even already distilled twice in vacuo, and thats all what he got out.
So thats just eight times your products volume, made from twenty times of what your substrate weighed.
Although yours sounds like it was superior bark mostly and not whole chipped roots.

Besides this, nice and interesting piece of work.
You really should take a look into the mentioned thread, and all the other pieces of work from the same person(actually his neighbor), they all start with the isolation of ethereal oils and how to process each of them to the respective final product.


Yes, I’ve read all about the thread you mention. It was partly my inspiration for the project. Right now I’m processing some root bark to determine the oil content of the roots I’m using so i can get an estimate on how much fresh root bark is needed to get the amount of oil i to do any further processing ;)

Ill update with picture in a few minutes to show you some of the things I’ve been talking about. Hang tight.

chemist1243 - 20-10-2020 at 18:50

Update: a few pics of the process

In one of the pics you see a flask with tin foil and part of the distillation head attached. This is the insulation that i find works well for this project. In another photo you see a 500ml beaker with brown stuff in it, this is the root bark sludge. The last photo i posted is an opaque liquid sitting in a beaker. If you look close, you can see a few globules of oil scattered around. This is sassafras oil, and I’m gonna take a guess and say that it’s at least 60% safrole, however I’ve heard people say that they have distilled oil from North American trees as low as 50%.

Like i said in another one of my posts, ill have and update with the essential oil content of the root bark i used(125g of fleshy soft root bark).

If you are actually planning on doing this, here’s a few quirks you may run into:

1: if the sludge doesnt pour into the neck of a 24/40 flask without spillage, cut off the top of one of those flimsy water bottles and use it as a funnel. Glass funnels can’t be used because their stem is too thin. Same thing with most kitchen funnels. This improv funnel wont fit all the way but it’ll fit just enough to not have any leakage.

2: “the oil bath stinks and the hydrosol/oil doesn’t smell like the roots or like sassafras at all”. First of all, if your oil bath stinks, the oil could be burning, and also when using peanut or vegetable oil it stinks like that anyways, so just turn the fan or fume hood on and suck it up. Dont worry about the smell of anything until you’ve separated the sassafras oil and dried it. If you Let it sit for a few days the smell becomes much more strong than when it was first dried and collected. Like karlos said, the hydrosol it useless, although in my personal experience i find that after leaving it to sit for a few days it did clear up a bit and i got a few tiny globs of oil at the bottom. Not enough to matter, though.

3: “how do i tell if what i have is root bark or inner root?”. Root bark from a freshly killed tree peels away from the rest of the root like an orange, leaving a slightly slimy layer where the root bark used to be. The root bark can always be broken by the hands when at room temperature, however the root cannot, its fibrous and tough and can give splinters just like wood from the trunk, although the root is still very fragrant and can be used for tea and whatnot. Just make sure to not use it for this procedure. If you do you’ll end up getting no useful amount of oil. Besides, root bark is easier to break up. Now, if you wanna bring in a 500 liter liter pot still you welded from say, a cut in half propane tank, sheet metal, and some piping, then go get yourself a wood chipper and process the roots and the rootbark, thats how its done nowadays for all the people looking to have some real fun ;)


And most importantly: dont get caught in the idea of making a whole boat load of sassafras oil. This is for someone who doesnt really have the space, skills, time, or money to build a proper multiple hundred liter distillation tank, but who may have a little forest to play around in - like me.

I have conceived this prep in my mind since the day i realized how hard it is to find legit oil. Now i can get all i need using minimal equipment. Maybe i did have that tractor, but I’ve also used a hatchet and shovel and that’s worked okay, too, so dont be discouraged.

Once you have the sassafras oil, go find one of the various archived guides on how to refine it into pure safrole. Once you do that, then the chemistry really starts. :D

Or you could, y’know, use it in perfume or something. Not my type of fun, but its yours to do whatever you want with.








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zed - 21-10-2020 at 03:59

Well, folks may be poaching trees out in the wild. But, it is a minor percentage of world use.

I would imagine most of the world's output goes to make insecticides, or Heliotropin.

The Heliotropin, can be used as a scent, to make ice cream, or in the synthesis of the ever popular Cialis.

I'm thinking that the world's output of Cialis, is greater than its output of X.

[Edited on 21-10-2020 by zed]

karlos³ - 21-10-2020 at 05:43

Quote: Originally posted by zed  

I'm thinking that the world's output of Cialis, is greater than its output of X.

I remain still somewhat doubtful about.
Cialis got quite popular even under younger people who don't need it at all(but it is still great, no doubt), and under that part of the population, taking both isn't uncommon.

Now lets do the math, cialis 20mg, that should suffice well.
But MDMA? People take somewhere between 6-10x as much(ok we're talking about men only, lets say 8-12x as much), and then consider the mass of piperonal in tadalafil and the mass of the piperonal moiety in MDMA.
Cialis is taken in much lower amounts, and, I estimate now, consists only to ~1/4th out of piperonal,
MDMA is taken in ten times as large amounts, and consists to around ~1/2 out of the piperonal moiety.

I am not sure that people really use more of the latter, but neither convinced of cialis being the leader of that race, and if definitely not with a huge advance.
It could be really close I would think.
Definitely if we judge on which drug uses up more piperonal, although its obviously problematic with one of them being produced illegaly.

But if you meant with output the number of produced pills... well then its clearly cialis, no doubt about this :P

Corrosive Joeseph - 21-10-2020 at 06:17

Quote:


Tadalafil was approved for medical use in the United States in 2003. It is available as a generic medication in the United States and United Kingdom. In 2017, it was the 282nd most commonly prescribed medication in the United States, with more than one million prescriptions.



I don't know about the US, but where I live, doctors will not prescribe more than 4 pills per prescription.

And when I was younger, it was estimtaed that 1 million ecstacy tablets were being dropped every weekend in the UK alone (population, about 50 million)

I would guess ecstacy is not nearly as popular as it was back then, and nor is it in the US, although, 20 years later, there are more people in the world. Pandemic aside, and given 'normal' conditions, I would say waaaay more E's are dropped than Cialis.


/CJ

chemist1243 - 21-10-2020 at 08:04





I’d say the world definitely uses more MDMA than any safrole derived LEGAL medications. By a long shot.

Remember that the market for MDMA is extremely lucrative, and the demand is higher than ever. It can be produced in mass quantities and is shipped all over the world. MDMA production, distribution, and usage doesnt have to abide by government standards in the way that legal medications do.

You cant simply ship however much medication you want anywhere to anyone in any quantity. It’s regulated, recorded, and inspected. With MDMA people use however much they want whenever they want, they aren’t bound by prescription limits.

It’s tempting to say that interception of shipments combats this, but the reality is that as agents inspecting mail high five eachother over a 100 kilogram seizure, 10 times that probably slips right past.

There’s no stopping the drug trade, it just keeps on chugging along with a momentum that only the ignorant believe can be slowed. Even the biggest of busts only slow it down by the amount a penny on a railroad track would slow down a freight train going full speed

[Edited on 21-10-2020 by chemist1243]

ChemichaelRXN - 21-10-2020 at 08:12

MDMA is great, but it isnt worth risking your life over. There are many other compounds out there. Unless you are set up for large scale synthesis, you wont make much money anyway. Look into methylone if it is legal where you are. They are pretty similar and you can import kilograms for a few thousand. I prefer MDA much more over MDMA. I had the best experience of my life on MDA.

Anyway, have you considered the piperonal route over killing a ton of sassafras trees for a few drops? You can import the 3,4-dihydroxybenzaldehyde for very cheap.

That is a good yield of the oil though. Must have been very oily.

All the best and be careful!

[Edited on 21-10-2020 by ChemichaelRXN]

chemist1243 - 21-10-2020 at 08:32

I agree. You should risk your freedom and life for nothing. I see pure MDMA as a relatively safe compound, however it defiantly can spiral into a crippling addiction or worse. As always, use caution whenever trying out any substance - legal or not.

Regarding the piperonal routes, while agree mass deforestation is a huge negative consequence of MDMA production, i simply cant help but disagree on the route. safrole is just the number 1 best precursor for MDMA. It’s extremely notorious for its reliability, high yields, and ease.

You cant expect people to switch to a route which is almost never talked about and even more rarely put to practice or written about. Besides, sassafras grows like weeds where i live, so its not really like I’m degrading an entire ecosystem of endangered trees. In fact I’d say i did less harm to the environment getting that rootbark than i would’ve done buying dihydroxy benzaldehyde from a manufacturer who is slowly polluting the environment by industrial production.

Update

chemist1243 - 21-10-2020 at 11:29

Ive had a minor set back in determining the oil content of my rootbark. I spilled some oil, so i have to redo the experiment if i want accurate results. I was hoping to finish up by tommorow however now I’m thinking its gonna be more like Friday or Saturday.

I apologize to anyone who was eager to hear the results.

Texium (zts16) - 21-10-2020 at 19:57

You should try extracting the hydrosol with ether after collecting the oil droplets. You could probably increase your yield a little that way.

Cou - 21-10-2020 at 22:28

Quote: Originally posted by chemist1243  
I agree. You should risk your freedom and life for nothing.


Do not give the evil rich people the satisfaction of being a helpless prison slave. Do not give the cops their sick satisfaction of handcuffing a helpless kid. The best time to use illegal drugs is when you're a terminal illness patient or getting old and close to death, in which case you won't live to suffer the legal consequences anyway.

[Edited on 10-22-2020 by Cou]

B(a)P - 22-10-2020 at 03:24

Quote: Originally posted by ChemichaelRXN  
MDMA is great, but it isnt worth risking your life over.
[Edited on 21-10-2020 by ChemichaelRXN]


I would like to start by saying my organic chemistry knowledge is embarrassingly lacking, so forgive my uninformed questions.
As a reagent, does sassafras oil have a use other than the production of MDMA?
I am curious, because I have seen a few posts where it is sort after, including this one and the end goal isn't really described.

chemist1243 - 22-10-2020 at 05:51

Excellent question. Safrole is a precursor to many pharmaceuticals like the aforementioned talafadil, and its also used to make pesticides like piperonal butoxide. Most of the time the starting chemical is not safrole, but actually piperonal which is made from safrole.

Sadly, due to MDMA production combined with industrial demand for piperonal-based pesticides, the sassafras tree native to many south East Asian countries is slowly going extinct.

Hopefully ways to make piperonal synthetically such as the dihydroxy benzaldehyde route will be studied and optimized to be easy and cheap in the near future, but even then you’d still have people cutting down the trees for MDMA.

This isn’t a drug synthesis fourm, so i dont want to muck up the waters for myself talking about my intentions. Let’s just say the safrole i have wont end up in rave or traded for money, but more likely in a sealed vial in a locked box along side other sealed vials. The end goal isn’t the substance, its the feeling you get from making everything work using minimal resources, thats the high that I’ve been chasing for the longest time now.

[Edited on 22-10-2020 by chemist1243]

zed - 22-10-2020 at 11:55

Well pirating trees in the rainforest is popular in third world countries. It damages the forests and may be threatening extinctions. I don't know. It is a source of spot-cash-money, for folks that are desparately poor. To them, it's just some tree in the forest, while their children at home are hungry and need to eat.

But, Cinnamomum Camphora, is in no danger in the U.S.. It is fairly common, and it is considered an invasive species. Go to Southern California, Texas, or Florida... Lots of trees. The percentage of safrole in the wood is small, but an older tree weighs thousands and thousands of pounds.

As for Safrole being the most straight-forward route to the ketone... No, I don't believe that is necessarily
true. But, Heliotropin and Nitroethane, are far more difficult to acquire.

chemist1243 - 22-10-2020 at 12:17

Well, your right. Most of these people are not hardened criminals, they are just poor workers trying to support a life for their family while being exploited and underpayed by the criminal organizations who employ them. A large amount of safrole for MDMA production actually is from camphor trees, particularly “brown camphor oil” which is the safrole fraction of camphor wood oil. This camphor oil comes from Asia though, not the south.

On a lighter note, I’m almost finished distilling the bark, and i may even be able to post yield results by tonight. No promises, but I’m very close. Ill update when its ready.


UPDATE: results

chemist1243 - 22-10-2020 at 13:39


Starting amount: 112g of fleshy moist sassafras rootbark
Yield of sassafras oil: 2.2g
% yield: 1.96%

Commentary:

The yield is only about 2% before drying. Pretty shabby, but thats the way it is. The oil from this batch was much more viscous than my last batch. It was closer in consistency to olive oil or vegetable oil than the sassafras oil i know and love.

You can see in one of the photos i attach, the is clumps of oily solid. That’s what it looks like when drying micro quantities of oil, its just painful to look at all the oil left behind and lost. You could just make the whole thing an acetone solution, but thats no fun. This oil loss is why its more efficient to save up a lot of undried oil and then dry it all together. You’ll lose a lot if you dont. Then again, drying is optional but preferred.

If you oil is cloudy like mine in the other photo, then you got some magnesium sulfate still in there from the drying step. Vacuum filtration would probably be best to remove this.



Now my whole lab smells like sassafras :D



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Texium (zts16) - 22-10-2020 at 13:59

Why not extract with ether, dry the ethereal solution, then decant and evaporate? You’ll lose a lot less oil that way since whatever liquid is left stuck to the drying agent will be some % of oil in ether instead of 100% oil.

And to reiterate my earlier question since it was not answered, did you try extracting the hydrosol to recover more oil? I’m curious to see how much this would increase your yield.

brubei - 22-10-2020 at 14:16

Quote: Originally posted by B(a)P  
As a reagent, does sassafras oil have a use other than the production of MDMA?
MD-benzyl is common building block in drug design. Just go to aldrich or other chem seller an search for substructure like it, you'll find plenty of results.

drugbank.com find 77 products, marketed pharmaceuticals or pharmacological compound with this moiety.

chemist1243 - 22-10-2020 at 18:17

Quote: Originally posted by Texium (zts16)  
Why not extract with ether, dry the ethereal solution, then decant and evaporate? You’ll lose a lot less oil that way since whatever liquid is left stuck to the drying agent will be some % of oil in ether instead of 100% oil.

And to reiterate my earlier question since it was not answered, did you try extracting the hydrosol to recover more oil? I’m curious to see how much this would increase your yield.


No, i have not tried any ways to recover any oil from the hydrosol that may be lost. To me, it is not worth the effort for such a small amount of oil gained in return. I would be glad to send you some sassafras hydrosol if you are willing to experiment with it and post the results yourself, though.

As for the drying step; it wont hurt your yield much as long as you’re drying >10ml quantities of oil. I measured the oils weight before drying, so actually the yield i measured is theoretically too high, but only by 10’s of milligrams.





Mateo_swe - 25-10-2020 at 09:07

If one where to increase yields by extracting the hydrosol, what solvent would be best to try?
Not only safrole, for most aromatic essential oils that are extracted by steam distillation.
Would DCM work good for hydrosol extraction?
Its low boiling point make it easily removed and i have some of it i can use.

Antigua - 25-10-2020 at 09:13

Chloroform, DCM, diethyl ether would all work. Safrole is miscible with pretty much all organic non-polar solvents. DCM could prove a little tricky as it tends to form emultions sometimes, but provided you have a way to deal with it (usually a bit of brine and time) it's suitable. In one episode of Hamilton's Pharmacopeia the chemists used a... vibrator. Whatever works.

karlos³ - 25-10-2020 at 11:41

I repeat, extracting the hydrosol is not worth it, its too bad soluble in water.

chemist1234, you keep talking about deforestation regarding piperonal.
I may be wrong, but I am quite sure that most of the piperonal used in the industry today is made from lignin, similar to vanillin.
They go in that case via catechol I think, which really is a dirt cheap process.

The stuff made from isosafrole, pepper or whatever, is opposed to this much more expensive, but those who use this in their products do so because they can write "made from 100% natural ingredients" according to customer protection laws on their products, giving them a huge increase in sales and thus worth to them to be used instead of the cheap material.

So, piperonal comes not from deforestation, but from deforestation(of any kind of trees) comes piperonal(and vanillin and so on).

arkoma - 25-10-2020 at 15:11

Karlos3, I imagine the OP was thinking of the havoc done this tree in Cambodia.

karlos³ - 25-10-2020 at 23:08

Ouch! They throw everything together in this article, speak of a rare tree which camphor isn't, of sassafras oil which is wrong too, and so on...

Mateo_swe - 26-10-2020 at 10:11

But the common Cinnamon camphora tree dont have a high% safrole.
Cinnamon camphora is a quite common tree growing in many parts of the world.
Its the high yielding cinnamon variants that are harvested and becoming very rare now.

Mateo_swe - 26-10-2020 at 11:39

Quote: Originally posted by karlos³  
I repeat, extracting the hydrosol is not worth it, its too bad soluble in water.

Is that so for the hydrosol of other phenylpropanoids too or just in the case of safrole?

chemist1243 - 28-10-2020 at 11:16

Quote: Originally posted by Mateo_swe  
Quote: Originally posted by karlos³  
I repeat, extracting the hydrosol is not worth it, its too bad soluble in water.

Is that so for the hydrosol of other phenylpropanoids too or just in the case of safrole?


Look up the solubility of said phenylpropanoid(aka; UTFSE) and you’ll find out. :)

Texium (zts16) - 28-10-2020 at 11:32

The solubility isn’t the only relevant factor. If your hydrosol is cloudy then you have an emulsion, and there is probably more oil hiding in there than you would expect to be soluble, as microscopic, immiscible droplets.

Maybe it still wouldn’t be a significant amount, but it would be nice to see someone try it. With other essential oils I have extracted that are practically insoluble in water, such as limonene, it has helped significantly.

ChemichaelRXN - 28-10-2020 at 22:09

I dont do anything with anything scheduled, but if you were to get every last drop, Id extract the steam distillate with chloroform and then rotovap it. Not worth it to make anything illegal for me because I am an innovator and come up with new compounds. Every so often you can find these rotovaps for incredibly cheap...i think I only paid 145CAD for my first one and it came with a condenser surprisingly. You can make a setup like this and they are very handy for the odd project.

I was doing a reaction recently with DCC as the catalyst and joining GABA and phenethylamine to form an amide. Called N-GABA-phenethylamine...maybe I will make another thread about it. Not sure about bioactivity...just for research.

648981C1-9873-4B82-B5A8-357E8F408027.jpeg - 86kB

chemist1243 - 29-10-2020 at 06:57

That is incredible work. I’m not skilled enough to synthesize organic compounds like these by myself, but I aspire to one day be able to. As insignificant as it may be from someone like me, I’d like to say that I have a lot of respect for this kind of chemistry. Bravo, Sir!

ChemichaelRXN - 29-10-2020 at 09:16

Thanks, I appreciate it. I strive to do more, but I am usually in a state of feeling miserable from a heavy buzzing in the mind and other symptoms. (Glad I can work from my home office at least or I’d be on disability.) Lets hope XRP goes up in value and maybe I can retire early...I am sure as f*** i wont get a dollar from some group of parasites that attacked me when younger and took my intellectual property. Lol

Anyway, the sassafras root makes a nice aromatic pendant too...just an idea. (Sort of like an accolade)

Back on topic...sorry!


[Edited on 29-10-2020 by ChemichaelRXN]

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Mateo_swe - 2-11-2020 at 12:47

Im trying an experiment and see if i can get some safrole oil out of dried leaves from my Piper Auritum plants.
The leaves have been saved as they fall off since spring and were dried but they still smell strongly of licorice so i thought it might be worth a try.
I crushed the leaves in a big clay mortar and pestle thing and the licorice smell was very strong, made me sneeze repeatedly.
I managed to get 130 grams of dry leaf material that i hydro distilled with an attached clevenger device.
To my disappointment i managed only to get very little oil, i guess maybe 2 grams/ml.
It smells strongly of a smell that could potentially be root-beer or safrole. I have never tasted or smelled root beer nor have i smelled the aroma of safrole before.
Its a too small volume for any fractional distillation so i will save it and try another steam distillation when i saved up some more leaf material.
This time i think i put the leaves in the freezer after they fall to better preserve the oil.
Piper Auritum leaf oil have between 65 to 93% safrole content according to included paper and the fresh leaves have about 0.2% oil.
The grow conditions probably matter a lot and i have no clue if drying the leaves is bad or if it doesnt matter.
From my results it seems drying the leaves isnt good.

Attachment: Essential Oils from Neotropical Piper Species and Their Biological Activities.pdf (3.7MB)
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karlos³ - 2-11-2020 at 13:43

You're familiar with this thread?
Here: http://www.sciencemadness.org/talk/viewthread.php?tid=90636
2g is around that what I would have expected from that quantity of plant material ;)

Mateo_swe - 4-11-2020 at 12:55

I have seen that thread but not before i started the experiment.
I thought there would be more than 2grams from that material but it seem to be around the same % that the other guy in the thread you linked above got too.
There is a better Piper variant but its rare.
Piper aduncum is quite common and maybe has more oil but has dillapiole not safrole.