Fluorination Kit

Fluorination Kit:
(HCK1008-01-001)

Fluorination is one of the most interesting C-H functionalization described in literature. Our kit is designed to conveniently screen fluorination reaction conditions using PdOAc2 as catalyst in presence of most common fluorine sources; Silver Fluoride AgF, 1-fluoro-2,4,6-trimethyl-pyridinium triflate (TMPyF), SelectFluor®, and N-fluorobenzenesulfonimide (NFSI)  and oxidant Bis(tertbutylcarbonyloxy iodobenzene (PhIOPiv).

Kit Contains PdOAc2 with either AgF, SelectFluor, NFSI or TMPyF with or without PhIOPiv as oxidant 24 reaction vials totals

Protocol: The typical protocol is performed at 0.05 mol/l concentration of substrate with four different fluorinating agents. When present, reaction includes 10 mol% catalyst and 2 equiv. of oxidant. Each kit contains two sets of reagents allowing the screening of two different solvents. Preferred solvents for the fluorination kit include a 5% isobutyronitrile (iPrCN)/dichloroethane mixture, dichloroethane, acetonitrile and dichloromethane. If low solubility of substrate is observed, it is possible to decrease substrate concentration by increasing the reaction volume while maintaining the stoichiometry of the reaction. Maximum volume for reaction vial is 200 µl.

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

The typical protocol is performed at 0.05 mol/l concentration of substrate with four different fluorinating agents. When present, reaction includes 10 mol% catalyst and 2 equiv. of oxidant.
Each kit contains two sets of reagents allowing the screening of two different solvents.  Preferred solvents for the fluorination kit include a 5% isobutyronitrile (iPrCN)/dichloroethane mixture, dichloroethane, acetonitrile and dichloromethane.
If low solubility of substrate is observed, 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

  • Prepare required volume of a 0.05 mol/L solution of substrate in reaction solvent. For example, 700 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.
  • Using a clean and dry syringe, add 50 µl of substrate solution to each vial.
  • Stir the reaction vials in the reaction block at desired temperature (for example: 60°C) for 12-24 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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