The following is a method I tried to separate Safrole from Sassafras oil, but when I tried to wash the oil layer with water I could not see any separation of layers, so I could not wash. Also, the recipe does not state how much water to use. Help....anyone????

Starting weight: 112 g sassafras oil

Placed 454g 28% Acetic Acid in a 2L Sep funnel. Added 112g Sassafras oil. Shook for 3 minutes, waited 15 min for layers to form. Separated layers, kept the bottom layer, threw away the top layer (acetic acid, eugenol & other solubles).

Here the recipe calls to wash the solution 2X with dH2O. No amount was stated so I used a equal amount of dH2O. I didn't get any separation. Can anyone give me some advice as to why I cannot get any separation> Or, how much water should I be washing my solution with? The following is the rest of the recipe:

Add 100g of denatured alcohol, no layer forms as the product is misible in ethanol. Add 20 grams of dH2O. This pulls the ethanol and other product into the top layer, bottom layer containing some ethanol and safrole. Separate layers, place bottom layer into a 2L beaker. Take the temp right to 234C. The ethanol and water come off <=100C... The safrole starts to boil @ 232C, then came to a full boil and maintained 234C. The product is yellow orange in color. (The chemist of this sythesis checked it with 5% NaOH solution to see if any eugenol was left behind, no preticipate formed)

As always, thanx guys!

Screw all that washing junk. I have two words for you, fractional distillation.

Madchemist:

Well, help me out on this one. What kind of condenser, or do you use a distilling column? Could I use a "Graham" Condenser? Thanx, man...your always lending a hand.

kpjr

Fractionation column (I think that is what it is called), sort of like the ones at the oil refinerys. I am about to abort on the sassafras oil anyway, been reading how to make MD-P2P from beta-nitroisosafrol. Which can be made from black pepper.

[This message has been edited by madchemist (edited 10-17-2000).]

which recipe are you refering to, if you dont mind me asking?

What are you referring to, the black pepper?

say where i live there are hundreds of sassafras plants growing all over. Can you extract oil off of these and what part of the plant do i use?

Acidmelt: Buy the book, Total Synthesis II by Strike...it has all the recipes you'll need, including the one on how to extract sassafrass oil from the plant.

By the way, if anyone is wondering about the above sythesis (from Total Sythesis II)...the book made a boo-boo. When you wash the Sassafras oil with 28% Acetic Acid, instead of keeping the bottom layer as the book asks, we should be retaining the top layer of oil. That's why I couldn't see any layer forming in the next step, because water is miscible in Acetic Acid and Eugenol. But when you wash the top layer of the first step...separation is highly visible. Tried this last night (since this was my first time purifying sassafras oil, actually second including the screw up above) got through the whole synth, safrole's temp went right up to 234C and stayed...removed from heat and when the safrole cooled I hit it with a 5% NaOH solution and no participate formed.

What a shitty thing to deal with for a first timer like myself. I love the book, but you'd think that people would proof read it enough so there wouldn't be any mistakes like that!

I found 16 oz bottles of sassafras oil for 29.00. Just look for some hick stick herb farm or something. They may have to order it but so what....that's what I did.

You may look into a mirror and learn about yourself, or you can look through a window and learn about the world.

[This message has been edited by kpjr (edited 10-18-2000).]

kpjr- was that the only missprint you found during your synth? how much $ do you think you invested your first time - what kind of yeild did you get ? - does that book have pictures or graphics to help us challenged people out? (sorr so many ?'s).... I dont have the money to waste so I want to get as close as I can the first time around, dig? thanks.....101 (ps. thanks madchemist for all your help too)

No prob. Sasss oil can be removed by steam distillation.

I found a place that sells sassafas for 3.00 an ounce- is this what I should start with? How much if so should I pick up?

If you want to use sass oil then yes, get as much as you can!

Rabbit... So far in the book I have found 2 errors. One did not aply to me and was probably a type o, but could certainly foul things up for a novice, like myself. I have only got to the sassafras purification process...I am waiting for a Palladium Catalyst for my next reaction of safrole to MD-P2P. And as far as how much money did I spend on the first couple mistakes. Really, not much...I just wasted approx 400 ml of sassafras oil. Washing the safrole from the sassafras oil is really very simple...I mean very simple. But then again, madchemist has some great ideas too...some that are just as easy. Anyhow, I am probably not the person to ask to many chemistry questions, since I am only 2 months old or so when it come to chemistry. Although, I did spend alot of time (6 months) reading books on the subject. I think that's what anyone should do before they try to teach themselves somethin, ta know. Another great beginner chemistry book to start with is "The Organic Chem Lab Survival Manual", by James Zurbrick (Barnes & Noble). It fills you in on all the chem jargon that is sometimes impossible to decipher without chem knowledge. Anyway, I hope things go well for you. Good Luck.

Hey Mad(man)chemist:

Do you know of any links using Palladium Acetate and Tert-Butyl Alcohol in a reaction to make MD-P2P from safrole? I have a synth in this book, but the author states that up until it's publication in 1999, that the "ball was still up in the air on this one." The recipe I have was originally posted by someone named TDK from the HIVE. Any ideas?

kpjr

I'll check.
Here is a wacker oxidation using palladium: http://rhodium.lycaeum.org/chemistry/wacker.nitrite.txt
That is about all I can find for now. But I will get back to you if I find something else.

[This message has been edited by madchemist (edited 21-10-2000).]

[This message has been edited by madchemist (edited 21-10-2000).]

Thanx, bro!

kpjr