1,2-Dichloroethane → HCID 178445684, compound

Participants

Reaction Steps

To a solution of the intermediate from step F (90 mg, 0.175 mmol) in DMF was added HOAt (36 mg, 0.26 mmol), DIEA (92 μL, 0.52 mmol), amino tetrazole (45 mg, 0.52 mmol) and EDC (50 mg, 0.26 mmol). The reaction was left stirring at room temperature for 18 hours. The reaction mixture was diluted with ethyl acetate (20 mL) and washed with 1N HCl. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified on the Gilson reverse phase HPLC to give the title compound. 1H NMR (DMSO, 500 MHz): 8.42 (d, J=8.0 Hz, 1H), 8.03 (d, J=8.2 Hz, 2H), 7.68 (dd, J=6.6, 8.7 Hz, 2H), 7.39 (s, 1H), 7.35 (d, J=8.3 Hz, 2H), 5.81 (s, 2H), 3.63 (m, 1H), 1.87 (d, J=10.9 Hz, 2H), 1.76 (d, J=11.7 Hz, 2H), 1.2-1.0 (m, 4H), 0.83 (s, 9H). LC-MS: 2.50 min; (M+H)=581.3.

Provenance & Evidence