newbies - 17-2-2012 at 08:16
Hi I tried an epoxidation of isosafrole by the peracetic acid but it failed, the color of the solution didn't change and the peracetic acid seems to
not be really mixed with the isosafrole+DCM and I put the stirrer on a long time.
To make the peracetic acid I used:
-acetic acid GPC minimum assay > 98% 55,8ml
-H2O2 35% 55,2 ml
-H2S04 96% 0,66 ml
Could you help me or know what is the problem ??
Thanks.
GreenD - 17-2-2012 at 08:44
Where'd you get the isosafrole?
How old was the H2O2 - this has a shelf life.
Beyond that, not familiar with epoxidations, but I thought you had to reflux.
turd - 17-2-2012 at 08:58
If you want help you will need to describe exactly what you did. How did you prepare the peracetic acid, etc. Why did you not use the NaHCO3
"buffered" method? As it stands, your post is completely useless.
newbies - 17-2-2012 at 09:05
I made it by isomerisation of safrole. No I didn't have to reflux it but normaly peroxidation is an exothermic reaction and I have to be careful: the
solution not rise over 40°C but there isn't any reaction and i search why ?
I mixed together
-55,8ml of 99-100% glacial acetic acid
-55,2 ml hydrogenperoxide 35%
-0,66 ml sulfuric acid 96%
Then I take 33mL of isosafrole and mixed it with 51 mL DCM in an RBF with magnetic strring.After I add really slowly with the help of an addition
funnel the peracetic acid to the isosafrole+DCM with the magnetic stirring.
ScienceSquirrel - 17-2-2012 at 09:07
Thread moved because of insufficient information. Is this a known procedure or are you flying by the seat of your pants?
turd - 17-2-2012 at 09:25
What method are you following or are you improvising??
This here:
http://www.erowid.org/archive/rhodium/chemistry/peracetic.ch...
clearly says that the peracid does not form immediately. Did you let your acid alter? If yes, why didn't you say so, if no, why didn't you follow the
published procedures?
And GreenD is probably talking about the hydrolysis step.
Edit: Oh, and how do you know that it doesn't react - colours mean nothing.
[Edited on 17-2-2012 by turd]
GreenD - 17-2-2012 at 09:33
Where did you get the safrole, lol
I don't want to impose on your sources, but "safrole" isn't always safrole.
newbies - 17-2-2012 at 10:39
I let the peracid react during 4 days swirling it a couple of time everyday.
Normally the color have to change but it's the first time I do that so I don't know.
GreenD I distilled the safrole from sassafras oil.
[Edited on 17-2-2012 by newbies]