Cesium carbonate → HCID 68425331, compound

Participants

Reaction Steps

To a solution of the intermediate from step C (522 mg, 1.66 mmol) in DMF (10 mL) was added the intermediate from step D (460 mg, 2.0 mmol), followed by cesium carbonate (815 mg, 2.5 mmol). After stirring the reaction at room temperature for 3 hours, it was quenched by adding water and extracting with ethyl acetate (3×). The organic layer was washed with brine and dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography using 30% ethyl acetate-hexanes. 1H NMR (CDCl3, 500 MHz): 9.21 (d, J=2.1 Hz, 1H), 8.25 (dd, J=2.2, 8.2 Hz, 1H), 7.97 (d, J=1.8 Hz, 1H), 7.69 (dd, J=2.1, 8.3 Hz, 1H), 7.5 (d, J=8.2 Hz, 1H), 7.18 (s, 1H), 6.95 (d, J=8.2 Hz, 1H), 6.01 (s, 2H), 3.97 (s, 3H), 1.53 (s, 9H). LC-MS: 2.87 min; (M+H−56)=406.0.

Provenance & Evidence