Could anyone possibly help me with mabey a skeleton procedural for the top abstact for producing protocatechualdehyde from pyrocatechol.I would like to try this possibly,I'm a newbee so that abstact kinda leaves me in the dark but this is what I'd do if for some reason I absolutely had to without anything else to go on(or a clue what i'm doing)
Prepare a solution of 150g. catechol dissolved in 200ml dh20 and pour into addition funnel.In a 3-neck 2000ml fbf is placed??250g.glyoxylic acid in 500ml 10%NaOH solution?? then add 8g. aluminum oxide(that would be my choice if all are equal)and add reflux condenser(I don't think a condenser is needed none of the rxn components have b.p's below 50
c?)the other two necks are plugged with (1)a thermometer submerged in the flask contents to monitor temp.
(2)the addition funnel with catechol/dH
2O solution
contents of addition funnel added at a rate to keep the temp from rising above 50
c(also not sure if the additon is even needed,mabey just place the flask in a plastic tray and add the catechol all at once and then just add icewater as needed??)
Let this stir for??3hrs. after addition is complete??, unless rxn is still noticeably going then just let it stir until at least an hour after it has died down.
Totally lost here?guess i'd pour the contents of the rxn flask into a 25%NaOH solution stir the shit out of it for awhile and extract the whole shebang with Ether or DCM.
And if that didn't work next time i'd try a mild reflux for a few hrs with 25%NaOH solution.
And if that didn't work i'd try adding concentrated NaOH solution to the mix slowly and see what happens.
And if that didn't work.....well guess i'd bee screwed
.Any comments on any aspect of the reaction or any comments at all would be very appreciated,Thanks!
.Peace,Chambered.
Bee's don't die,we just multiply.