Safrole Isolation thru Freezing?

iodide · Sun Jun 19, 2005 8:04 pm

There is so much confusion (or perhaps personal variation) on this subject that all the posts I've read invariably result in contradiction regarding what is best to do.

Is anyone familiar with this process, and if so, is it possible to provide a simple-to-understand explanation of it. I understand that, generally speaking, it involves subjecting the sassafras to as cold as one can get it, with hopes of it freezing. But here's where I'm confused:

1. What exactly should be done if the damn thing doesn't freeze?

2. If it does freeze, won't it freeze solid? And if so, how is this useful in "separating" the safrole from the rest of the constituents?

If anyone can provide a simple mult-step explanation I'd be very grateful...

2spun · The Resistor

Iodide,

there is much info here and in the hive board on this matter, as well as the rhodium mirror

1. What exactly should be done if the damn thing doesn't freeze?

have you distill'd your sassoil to get safrole? try distilling 2 times.
if it does not freaze either your freezer needs to get cold'r or your safrole is not pure
as far as swiy knows

2. If it does freeze, won't it freeze solid?
i would hope that it would

And if so, how is this useful in "separating" the safrole from the rest of the constituents?

you should distill it for separating thats what swiy does anyway

If anyone can provide a simple mult-step explanation I'd be very grateful.

https://www.synthetikal.com/Rhodiums_pdfs/chemistry/index.html

https://www.synthetikal.com/Rhodiums_pdfs/chemistry/safrole.distillation.html

https://www.synthetikal.com/Rhodiums_pdfs/chemistry/safrole.congealing.html

https://synthetikal.com/synthforum/viewtopic.php?p=4481&highlight=#4481

there is much use your search skills, the above should cover it, swiy distill's his oil 2 times to get the purest he can get.

iodide · Sun Jun 19, 2005 10:40 pm

Thank you for the links.

However, I'm not sure why you recommend distillation of the sassafras oil to obtain the safrole before freezing it, when this method, If I'm correct, is precisely offered as an alternative to that - namely, a more attractive means of separating safrole out of the sassafras!

Perhaps you are using the freezing method to further purify your distilled safrole?

Soap · Sun Jun 19, 2005 11:45 pm

well when swim posted his pictures of his frozen safrole, he had also started an entire write up in html format. ill tell him to finish it tonight and post it. hopefully it will be of some use.

iodide · Sun Jun 19, 2005 11:47 pm

Excellent. Tell him that its much appreciated!

2spun · The Resistor

iodide,
However, I'm not sure why you recommend distillation of the sassafras oil to obtain the safrole before freezing it, when this method, If I'm correct, is precisely offered as an alternative to that - namely, a more attractive means of separating safrole out of the sassafras!

Perhaps you are using the freezing method to further purify your distilled safrole?

frist question- sassoil has more than just safrole in it as far as swiy knows.
as well swiy can put his sassafrass oil in the frez all day long and it won't frez.
distil'n seperates his safrole from the other (what ever) thats in the oil.

after a distill swiy's safrole will frez.

swiy use's the frez to see what hes got as far as safrole, if it's full of impurities swiy can't get nothing to freaze.

if iodides sassafrass oil frez's then thats great means that iodide has a high content of safrole in iodides sassafrass,
not the case in all sassafrass oil
as far as swiy knows anyway.
all good hope it helps some. swiy would be very happy if all his sassafrass oil would just frez,
but thats not been the case for swiy

iodide · Mon Jun 20, 2005 1:31 am

2spun,

Huh?

2spun · The Resistor

swiy
don't follow last question
iodide

methyl_ethyl · Riedel De Haen

As far as I know freezing the safrole out of sasafrass oil will not work unless your oil is of very high percentage safrole.

Also you don't want the temperature so low that the other components of the oil are at their freezing point or lower.

I think most folks freeze the oil in a glass beaker and scrape the bottom and sides of the beaker with a glass stirring rod to promote crystal growth. The use of a "seed crystal" (i.e. a frozen crystal of known highly pure safrole) also works very well from what I gather. It does appear that the safrole does need some "coaxing" in order to crystalize. So if you have highly pure sassy oil and you are not getting crystals, I suggest the use of a seed crystal (which you probably don't have) or freeze the oil in a glass beaker and scrape the sides as described above to "coax" the safrole to crystalize.

If done correctly this method can yield highly pure safrole that needs no further distillation prior to isomerization. That being said I would only perform this freezing method as a "first pass" purification, which would effectively reduce the volume that needs to be further distilled.

Please note I have never actually performed this procedure, it's much easier for me to just purchase isosafrole. LOL!!!!

I'm so spoiled, yes I know....

Hopefully soap's writeup will clarify things for you, and give you a visual representation of what things should look like.

Thanks Soap...

m_e

primathon · modified

From the hive thread 'cant get safrole? FREEZE IT!', which doesn't seem to be available online (that I've been able to find). Lots of good information, so I uploaded it here:

ApprenticeCook · DILLIGAF

Freezing should not replace distillation if you are conducting the isomerisation and peracid route, the wacker methods are far more forgiving on impurity levels.
For best results (this is what swim has seen done), take a small portion of sass oil and freeze it in the freezer to get a few seed crystals of pure'ish safrole, chill the rest of the bottle and use these seed crystals to freeze the rest of the safrole content, decant the remaining fluid from the bottle (leaving the pure'ish safrole solid) let this solid melt and repeat the freezing process again. Distill the final frozen content for the safrole fraction twice.

-AC

Soap · Mon Jun 20, 2005 11:11 am

swims apologies, he started and finished the davinci code today... highly recomended! the write up i made isnt much diffrent from info in this thread, and the thread that swim started not to long ago... (why the new thread btw???) swim didnt take any pics except for the one on "my" thread.
how do i post html documents?

TokenJ · Mon Jun 20, 2005 12:44 pm

Very shitty method freezing! I use that method to remove camphor to get brown camphor for distilation.

How you will get good product from not distilling is beyond me.

The_Dude · Mon Jun 20, 2005 2:18 pm

>How you will get good product from not distilling is beyond me.

Read the links provided by 2 spun and you will see why you had problems.

TokenJ · Mon Jun 20, 2005 2:52 pm

Ok im converted. i did try it when i was first starting out but it seems to me that it will only work with sassafras. what about camphor with a melting point of 179C,
or other safrole containing oils where the safrole content is low i have doughts about ther validation

any one out there that has used the freezing method on oils other than sassy?