Ethyl Acetate → HCID 10414074, compound

Participants

Reaction Steps

Treatment of 24 (0.25 g, 0.45 mmol) with LiBr (53 mg, 0.61 mmol) in EtOAc (50 mL) at 60° C. for 3 h, and chromatography of the product on silica gel, eluting with EtOAc/petroleum ether (from 2:1 to 1:0) gave IIb-13 (0.16 g, 66%): as yellow foam; 1H NMR [(CD3)2SO] δ 8.74 (d, J=2.8 Hz, 1 H), 8.73 (m, 1 H), 8.31 (d, J=2.8 Hz, 1 H), 4.28 (m, 2 H), 3.65-3.44 (m, 10 H), 3.13 (s, 3 H), 1.70 (m, 2 H); 13C NMR δ 165.1, 145.7, 145.4, 141.0, 136.2, 127.3, 122.1, 67.5, 58.4, 51.1, 36.7, 36.5, 31.7, 29.6. HRMS (FAB) Calcd. For C15H2279BrN4O9S [M+H+] m/z 513.0291. Found; 513.0281.

Provenance & Evidence