Ullmann Cross-Coupling Kit 본문
2 sets of Ullmann reaction conditions with CuI, 5 different ligands and 3 bases (K2CO3, K3PO4, and Cs2CO3). 36 reaction vials total.
The typical protocol is performed at 0.1 mol/l concentration reaction condition and 1 to 1 ratio substrates in 500 µl selected solvent. Resulting catalyst loading is 10%. 1.1 equivalents of base are preloaded (55 µmol). It is possible to decrease substrate concentration by increasing the reaction volume (see chart below). Maximum volume for reaction condition is 1000 µl. Recommended solvents are DMF, DMSO, Dioxane or ACN.
Protocol at 500 µl volume reaction condition
- Prepare required volume of a 0.1 mol/L solution of combined substrates in the desired sparged solvent. For example, 10 ml solution for 18 reaction conditions (1 ml extra to compensate potential evaporation).
- Using a clean and dry syringe, add 500 µl of substrates solution to each reagent vial containing the reagents. Shake the vial to allow reagents to mix properly.
- Stir the reaction vials in the reaction block at desired temperature (for example: 60°C) for 3 to 12 hours.
- Remove the vial caps.
- 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.
Ullmann Cross-Coupling Kit
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