HCID 86725315, compound → HCID 76684262, compound

Participants

Reaction Conditions

Reaction Steps

Into a glass vial, the product from step (c) in 2.5 ml acetic acid and 2.5 ml HBr (33% in acetic acid) was added. The stirred reaction mixture was heated at 60° C. for 6 hours. The reaction mixture was cooled and the volatiles were evaporated in vacuo. The residue was dissolved in water (25 ml) and washed with diethyl ether (3×). The aqueous layer was basified with 2M NaOH to pH 10 and extracted with DCM (3×). The combined DCM extracts were washed with brine, dried over Na2SO4, and solvent evaporated in vacuo to give the title compound as a colorless oil (35 mg). 1H NMR (300 MHz, CDCl3) δ 8.43-8.38 (m, 2H); 7.22-7.12 (m, 2H); 7.08-7.00 (m, 2H); 4.49 (dd, J=8.7 Hz, 2.7 Hz, 1H); 3.10-2.82 (m, 6H); 2.73-2.45 (m, 5H); 2.04-1.93 (m, 2H); MS: ESI (positive): 265 (M+1).

Provenance & Evidence