Sodium Carbonate → HCID 54747868, compound

Participants

Reaction Conditions

Reaction Steps

The product of Example 2 (2-1) (0.08 g, 0.16 mmol) was dissolved in DMA (2 mL) in a 10 mL reaction tube of a CEM Corporation Discover 300 Watt microwave reactor. An aq solution of Na2CO3 (2 M, 0.8 mL, 1.6 mmol), 4-tolylboronic acid (40 mg, 0.29 mmol) and bis(triphenylphosphine)palladium(II) chloride (11 mg, 0.016 mmol) were added and the tube was purged with nitrogen, capped and inserted into the microwave reactor. It was heated at 115° C., 50 watts maximum power, for 15 min. The reaction was diluted with EtOAc, washed with 2 M HCl, dried (Na2SO4), filtered and concentrated. The residue was purified by semi-preparative reverse phase HPLC on a C18 column eluted with 0-100% MeCN in water. The desired fractions were concentrated, dissolved in EtOAc and washed with water. The organic layer was dried (Na2SO4), filtered and concentrated affording the title compound (25-1). 450.9 (M+1); Rt=3.52 min.

Provenance & Evidence