Potassium Phosphate, Tribasic → HCID 67185398, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of Example 292 (100 mg, 0.227 mmol) in THF (3 mL) and water (1 mL) was added tetra-n-butylammonium bromide (146 mg, 0.454 mmol), potassium phosphate (144 mg, 0.681 mmol), 5-bromopyrimidine-2-carboxylic acid (70 mg, 0.34 mmol) and tetrakis(triphenylphosphine)palladium(0) (20 mg, 0.017 mmol). The reaction was heated at 120° C. under microwave irradiation for 30 minutes then cooled to r.t. The mixture was partitioned between DCM (50 mL) and water (50 mL). The aqueous phase was acidified with 1M HCl and the resulting precipitate was collected, washed with water (2×10 mL), Et2O (3×10 mL) and dried in vacuo to yield the title compound (16 mg, 16%) as an off-white solid. δH (CD3OD) 9.06 (2H, br s), 8.57 (1H, br. s), 7.32 (1H, s), 7.31 (1H, d, J 8.5 Hz), 7.07 (1H, d, J 8.5 Hz), 4.41-4.34 (2H, m), 4.07-4.01 (2H, m), 2.83 (2H, s), 1.34 (6H, s). LCMS (ES+) 875.0 (2M+H)+, RT 2.43 minutes (Method 1).

Provenance & Evidence