Scale-Up Guide: Palladium Precatalyst Cross-Coupling Reaction Screening Kit

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Important Note

All of the catalysts used in the kit are sensitive to air and moisture in their commercially available form. Please see the catalyst MSDS or product detail page for details on handling and storage. To best enable scale-up success, the use of glove box is highly recommended. However, modified bench top techniques are provide below.

General Guidelines for Catalytic Reaction Scale-Up

  • Oven dry all glassware and stir bars
  • Preheat oil bath to avoid temperature spiking
  • Use dry, high purity reagents (and substrates)
  • Use unopened Sure/Seal™ anhydrous solvents (or newly degassed)
  • Keep reactions under an atmosphere of nitrogen
  • Purge needle/syringe with nitrogen prior to use

Example Experimental

All solids (base, substrates, catalyst) were weighed on a bench top balance and added to a cooled, oven dried flask1,2 equipped with an oven dried stir bar. The reaction was capped and then purged and backfilled with nitrogen (3x) with a nitrogen-fed manifold needle. Anhydrous solvent (SureSeal™ed and punctured with a nitrogen-fed manifold needle) was then added via syringe.  If a liquid bases was required, it was added as the final component via syringe. When all constituents were added, the nitrogen line was removed3 and the reaction allowed to stir at the required temperature for the duration of the reaction.

1See the Cross-Coupling Reaction Manual: Desk Reference and Cross-Coupling Quick Guide: Bench Reference for more detailed additional guidance and troubleshooting tips

2Reaction vials capable of being sealed with a microwave cap are very useful as well. By design, the caps do not need to be replaced once punctured.

3For higher temps, a reflux condenser operated under nitrogen can be used

Palladium Precatalyst Cross-Coupling Reaction Product List