Alkoxylation & Acetoxylation Kit

Alkoxylation & Acetoxylation Kit:

8 sets of 3 reaction conditions. 10 mol% PdOAc2, PhIOAc2 with 2 different salts CuOAc2 and Ag2CO3 (and no salt) to be used with 4 different solvents (MeOH, EtOH, IPrOH and AcOH) 24 reaction vials total.

The typical protocol is performed at 0.1 mol/l concentration reaction condition of substrate, 10 mol% catalyst and 1 equiv. of oxidant.  When present, there is 1 equiv. of salt. It is possible to decrease substrate concentration by increasing the reaction volume (see chart below) while maintaining the stoichiometry of the reaction. Maximum volume for reaction vial is 200 µl.

Protocol at 50 µl volume reaction condition

  1. Prepare required volume of a 0.2 mol/L solution of substrates in DMF. For example, 400 µl solution for 12 reaction conditions (100 µl extra to compensate potential evaporation).  If solubility of the substrate is an issue, refer to table below.
  2. Using a clean and dry syringe, add 25 ul of solvent (MeOH, EtOH, iPrOH or AcOH/Ac2O mix) to appropriate vial (3x for each solvent, 12 vials total).  Take care to avoid cross contamination between solvents. The remaining DMF solvent can be useful for cleaning syringe between solvents.
  3. Stir vials at RT for 60 seconds.
  4. Using a clean and dry syringe, add 25 µl of substrate DMF solution to each reaction vial.
  5. Stir the reaction vials in the reaction block at desired temperature (for example: 60°C) for 12-24 hours.
  6. Remove the vial caps using a decapper.
  7. Prepare analytical sample for each reaction condition with 5 µl sample diluted into 200 µl in either DMSO or water/acetonitrile 50/50.
  8. Analyze resulting analytical samples by LC/MS.

*Alternatively, if DMF is problematic for your substrate, you can prepare individual solutions of substrate in each reaction solvent.