Already been asked, but I feel this topic could use a thread to itself:
MW: H2O2(34g); C2H4O2(60g); isostuffrole(162.12g).
1mol H202 + 1mol C2H4O2 ---H2SO4---> 1mol C2H4O3 + 1mol H20
So, if using 30% solution of H2O2 (1.11g H2O2/2.6g H20), we would need 110ml (30ml H2O2/80ml H2O).
Now we have: 110ml H2O(30%) + 60g C2H4O2 ---> 76g C2H4O3.
The second oxidation goes:
1mol C2H4O3 + 1mol isostuffrole ---> 1mol stuffone.
So, the lesson learned here, only applicable if we lived in a perferct world, would be that for every 162g isostuffrole, you should use 110ml H2O2(30%) with 60g GAA, which is ~ 60ml. For every 100g stuffrole, we would need 68ml H2O2 with 37ml GAA.
It seems 1% catalyst suggested, but is this percent by weight or volume? Would assume weight, so it would be 1.2g per 114g GAA+H2O2, or 0.7 ml, correct?
Here's the experimental (GAA/H2O2 + 0.33%; H2SO4 + 100%):
180ml H2O2 (30%) added slowly (~15min) to 100ml GAA, with 3ml H2SO4. After stirring for 16hr, solution was slowly neutralized with 10g sodium bicarbonate. Next, 200g isostuffrone in 350ml DCM was slowly added to flask, and allowed to stir for 16hr.
Semtexium, if we choose to use acetone instead of DCM, what do you think of the GAA/H2O2 ratios? goiterjoe stated to me in a PM that Rhodium seems to have used Ritter's performic ratio in chems. He also stated that Ritter seems to look more for a resulting product than for a perfect equation when synthing.
When adding sodium bicarbonate, would it be best to add excess, making the solution basic, or just enough to neutralize?
A perfect ratio suggestion would gladly be tested by SWIP personally, and the results reported. Perhaps not enough H2O2 was used in the past, resulting in not enough peracetic acid being formed in the first place.
Watcha think?
PB
*Also, could someone tell me what size stir bar is used for a 1L RBF when distilling/isomerizing?