Buchwald Cross-Coupling HCK1004-01-015

2 sets of 16 reagent combinations in separated vial for strong base and premixed for weak base; 8 Catalysts (BrettPhosG2, RuPhosG2, XPhosG2, tBuXPhosG3, tBuBrettG3, Pd₂dba₃/ dppf, Pd(PtBu₃)₂ and Pd(OAc)₂/CataCXium® A) and 2 bases (NaOtBu and Cs₂CO₃) 32 reaction vials total.

This kit requires EvoluChem reaction block (HCK1006-01-002) included in the EvoluChem Starter Kit (HCK1006-01-001).

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

• Prepare required volume of a 0.15 mol/L solution of combined substrates in the desired sparged solvent. For example, 1700 µl solution for 16 reaction conditions (100 µl extra to compensate potential evaporation).
• For Cs2CO3 reaction conditions: Using a clean and dry syringe, add 100 µl of substrates solution to each reaction vial.
• For NaOtBu reaction conditions: Using a clean and dry syringe, add 100 µl of substrates solution to each reagent vial containing a catalyst. Stir to dissolve the precatalyst. Then transfer content of the catalyst vial to a reaction vial containing a strong base.
• Stir the reaction vials in the reaction block at desired temperature (for example: 80°C) for 3 to 12 hours.
• Remove the vial caps using a decapper.
• 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.