>ok, assuming you want to use MeOH, how much is needed?
These are the magic ratios I use (from Shulgin, I think):
glycol from 100mmol reaction (ie after extracting with DCM from a 16.2g isosafrole run)
25ml MeOH
120g 15% H2SO4 (18g H2SO4, 102g water)
Bring to a reflux, then hold for just over two hours with stirring. Cool, extract with DCM (3x20ml) and wash three times with 60ml of 5% NaOH. You can use up to 40ml of DCM for each extraction, but I've found it's not really needed.
>also, what temp would you run the hydrolysis?
At reflux (ie keep it boiling). I think it's about 80C.
>you need to use refluxing aparatus or lose the MeOH to evaporation.
>if you run it under ~65°C then does it still work?
Yes & who knows... why do it that way?
>it was nice to be able to use a large stainless pot for those large rearrangements
Without methanol, for this reaction to have any chance, you would need a lot of stirring. How did you stir through stainless steel?