This method is mentioned in Rhodium's p-benzo page (
https://www.thevespiary.org/rhodium/Rhodium/chemistry/benzoquinone.html
)
but TFSE doesn't turn up anyone ever using this method.
I trid to follow the synth to the letter: 24.4g hydroquinone and 345mg of NaNO2 suspended in 100mL technical grade DCM, the acetone/ice bath was kept up, along with magnetic stirring for 24 hours.
At the end, the DCM was transparent yellow, as expected, and dried for awhile in a homemade dessicator over Calcium Chloride, I left it in the dessicator and the DCM evap'd off quickly(I lost my vacuum adaptor so couldn't distill the DCM off).
Final yield was under 1 gram of pea green crystal shards, along with some black crystals assumed to be the quinhydrone .
Can anyone spot anything wrong?
I don't know if my ice bath got to -10°C, thermometers were in the mail at the time.
HCl used was 34% (w/w) muriatic acid from the hardware store. The oxygen was from a bottle for a torch.
Because of the reagents being so cheap I'll give this a try again soon and report back. Hopefully someone has some ideas or can spot my mistakes.
Thanks
blaaky