Ir/Ni Base and Ir Catalyst Screen Kit 1
2 sets of reaction conditions with 6 iridium catalysts Ir(dF-CF3–
This kit requires EvoluChem™ PhotoRedOx Box – HCK 1006-01-016 and EvoluChem™ Light Source 18W-450 nm – HCK 1012-01-002 as well as Syringe, decapper and reaction block included in the EvoluChem Starter Kit (HCK1006-01-001)
The typical protocol is performed at 0.05 mol/l using a solution containing two coupling components. Each sealed reaction vial contains 0.1 µmol of
Protocol at 100 µl volume reaction condition
- Prepare the required volume of substrate solution at 0.05 mol/L containing both coupling substrates. For example, 2.0 ml solution for 18 reaction conditions (200 µl extra to compensate potential evaporation).
- Degas substrate solution with subsurface sparging via N2 or Ar line with exit needle for 5 minutes.
- Using a clean and dry syringe, add 100 µl of the substrate solution to each reaction vial containing Cs2CO3 and
CsF(excluding DBU vials for now).***
- Add remaining 800 µl of substrate solution to
vialcontaining DBU. Stir and degas for 5 minutes.
- Transfer 100 µl substrate/DBU solution to each DBU reaction vial.
- Stir the reaction vials in the photochemical device for 18 to 24 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.
- Alternatively, reaction solvent can be evaporated in vacuo and
crudemixture diluted in water/acetonitrile prior to preparation of analyticalsample.
- Analyze resulting analytical samples by LC/MS.
***Alternatively, 2.24 µl of DBU can be added to each of the 6 DBU reactions separately using 10