2 set of 12 reaction conditions. 10 mol% PdOAc₂, 1 or 2 equivalents of PhIOAc₂with 5 different salts CuOAc₂, Ag₂CO₃, K₂CO₃, Cs₂CO₃, and MgSO₄ (and no salt).
24 reaction vials total

The typical protocol is performed at 0.1 mol/l concentration reaction condition of substrate, 10 mol% catalyst and 1 or 2 equiv. of oxidant.  When present, there is 1 equiv. of salt.It is possible to decrease substrate concentration by increasing the reaction volume while maintaining the stoichiometry of the reaction. Maximum volume for reaction vial is 200 µl.  The reaction is performed in the solvent of the desired transformation, (i.e. methanol for methoxylation), ethanol or isopropanol. For acetoxylation, use a 1:1 mixture of acetic acid and acetic anhydride as solvent.  If solubility is an issue, a 1:1 mixture of DMF and appropriate solvent can be used.

Protocol at 50 µl volume reaction condition

1. Prepare required volume of a 0.1 mol/L solution of substrates in appropriate solvent. For example, 700 µl solution for 12 reaction conditions (100 µl extra to compensate potential evaporation).  
2. Using a clean and dry syringe, add 50 µl of substrate solution to each reaction vial.
3. Stir the reaction vials in the reaction block at desired temperature (for example: 60°C) for 12-24 hours.
4. Remove the vial caps using a decapper.
5. Prepare analytical sample for each reaction condition with 5 µl sample diluted into 200 µl in either DMSO or water/acetonitrile 50/50.

Analyze resulting analytical samples by LC/MS.