Buchwald Cross-Coupling HCK1004-01-013

Buchwald Cross Coupling Array:
Pd Amination Strong Base Kit 6
(HCK1004-01-013)

2 sets of 24 reagent combinations in separated vials; 8 Catalysts (DavePhosG3, JackiePhosG3, JosiphosG3, P(t-Bu)3G4, PCy3G4, RockPhosG3, SPhosG3 and XantphosG3) and 3 bases (NaOtBu, LHMDS, and P2-Et) 48 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%. Each reaction contains 1.5 equiv. of base (22.5 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. (2.7 ml if performing reaction with 3 bases -100 µl extra per base to compensate potential evaporation).
  • Transfer 900 µl substrate solution to NaOtBu vial and mix.
  • Using a clean and dry syringe, add 100 µl of substrates/NaOTBu solution to each catalyst vial A1 through A8 containing a catalyst and a stir bar. Stir to dissolve the catalyst.
  • Transfer 900 µl substrate solution to LHDMS vial and mix.
  • Using a clean and dry syringe, add 100 µl of substrates/LHDMS solution to each catalyst vial B1 through B8 containing a catalyst and a stir bar. Stir to dissolve the catalyst.
  • Transfer 900 µl substrate solution to P2-Et vial and mix.
  • Using a clean and dry syringe, add 100 µl of substrates/P2-Et solution to each catalyst vial C1 through C8 containing a catalyst and a stir bar. Stir to dissolve the catalyst.
  • 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.

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