Buchwald Cross Coupling Array:
Pd Amination Weak Base Array
2 sets of 10 reagent combinations in separated vials; 5 Catalysts (BrettPhosG2, RuPhosG2, XPhosG2, tBuXPhosG3 and tBuBrettG3) and 2 bases (NaOtBu and LHMDS) 20 reaction vials total.
The typical protocol is performed at 0.15 mol/l concentration reaction condition and 1 to 1 ratio substrates in 100 µl selected solvent. Resulting catalyst loading is 10%. Two equivalents of base are preloaded (30 µmol). It is possible to decrease substrate concentration by increasing the reaction volume (see chart below). Maximum volume for reaction condition is 250 µl. Recommended solvents are dioxane, tBuOH or Toluene.
Protocol at 100 µl volume reaction condition
requiredvolume of a 0.15 mol/L solution of combined substrates in the desired sparged solvent. For example, 1100 µl solution for 10 reaction conditions (100 µl extra to compensate potential evaporation).
- Using a clean and dry syringe, add 100 µl of substrates solution to each reagent vial containing a
precatalyst. Stir to dissolve the precatalyst.
- Transfer content of the precatalyst vial to a reaction vial containing a strong base.
- Stir the reaction vials in the reaction block at
desiredtemperature (for example:80°C) for 3 to 12 hours.
- Remove the vial caps using a
analyticalsample 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.