Swim has a real big problem with chromic`s peracetic oxidation.
After trying to destill the desired ketone some colorless shit came over.
The boiling point was 98-100 C with vacuum. Safrole comes over at 90C at the same vac.
Ketone made via Benzo Wacker comes at 125-140 C and has a yellow colour, doesn´t freeze
and smells beautiful.
But this little piece of shit smells only a little bit after ISO and freezes at -16 C.
So what could that be Swim had produced?
Here my setup:
Cromic´s version was scaled down to the half of the org. amounts (26,35)
-ISO was made via KOH and heating at 150 C for 12 hours.
ISO came over at 105C at same vac as above. It smells less than Safrole.
-selfmade peracetic acid aged 12 days (instead 5-7) was used.
-Then dumping the acid into the DCM/ISO/NAHCO3 solution no warmup appeared.
Nevertheless the solution turnt into a light yellow after 5 hours.
But it was stirred another 4 hours due to no time to go on.
-After washing it with 5% NaOH the second wash ate a lot of the yellowish colour.
Swim was a litlle confused what there was happening but he went on.
-So the DCM was destilled off and the residue was reacted with 15% H2SO4
at reflux for 3 hours.
-Wash with DCM with a reddish colour change of the solvent
-Again washing 3 times with 5% NaOH. The first one ate nearly the whole reddish colour.
-Destilling off the DCM
-Then the shit (absolutly no ketone) came over at 98-100 C at vac.
So what the holy fuck can this be?
Maybe converted to some other shit? Alcohol?
Why does the NaOH eat nearly all of the yellow colour?
In this step the yellow colour indicates for the Epoxide, doesn`t it?
Another question?
Will in the fist step a yellow colour be formed even with plain Safrole?
Is the yellow colour an indication that the reaction went right?
Any bee who can help, please take the time....
Many thanks in advance.
The Hive with all of your bees is the best community
---THANKS FOR THAT in the name of holy Jesus Christ---