No, what I'm thinking is that this method tears apart the sassafras molecule... my guess (a complete hypothesis) is that it destroys the methylenedioxy bridge or *something*. When you go to the base wash, you get crap... kinda light brown chunks of insoluble stuff suspended in a black liquid between the two phases (maybe there is a lot of ketone in there, but I had no idea how to recover it). This is why I gave up with trying to get this method to work.
I don't believe the method does work for a lot of bees. I've heard other stories of failure. If you want a good, verified, peracetic method... use:
https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracetic.chromic.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracetic.chromic.html)
Enjoy! I'm sure your sassafras is good, but check it with all the standard tests. (search under my username)
https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracetic.chromic.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracetic.chromic.html)
^--- nice
Is 5 hours in the ice bath really necessary after adding in the peracetic acid in to your isosafrole?
G'job.
I totally looked over the peracetic method and was using formic acid like the black plague for few months. Halleluia.
This nice article has been referenced earlier in Post 245000 (https://www.thevespiary.org/talk/index.php?topic=7415.msg24500000#msg24500000)
(Greensnake: "preparation of peracid solutions", Chemistry Discourse)
Preparation of Aliphatic Peroxyacids
Benjamin Phillips, Paul S. Starcher, Bertrand D. Ash
J. Org. Chem. 23(12), 1823-1826 (1958) (https://www.thevespiary.org/rhodium/Rhodium/pdf/aliphatic.peroxyacid.preparation.pdf)
(https://www.thevespiary.org/rhodium/Rhodium/pdf/aliphatic.peroxyacid.preparation.pdf)
Abstract
Convenient procedures are described for preparing peracetic and perpropionic acids as anhydrous solutions in solvents of negligible acidity. The method is based on the reaction of carboxylic acids with hydrogen peroxide and employs azeotropic removal of water to drive the reaction to completion. Conditions for safe operation are chosen on the basis of measurements of the detonability of peracid solutions.