HCID 86713389, compound → HCID 86713390, compound

Participants

Reaction Steps

A mixture of Intermediate 37D (1.25 g, 3.53 mmol) and 10% Pd/C (200 mg, 0.188 mmol) in EtOAc (50 mL) was purged with hydrogen. The mixture was then stirred under a hydrogen atmosphere for 1.5 h. The suspension was filtered, and the filtrate was concentrated to dryness. The crude material was purified by flash chromatography (SiO2, 24 g column, EtOAc/hexane=0-40%) to afford Intermediate 37E (939 mg, 82%). HPLC: RT=2.986 min (CHROMOLITH® SpeedROD column 4 6×50 mm, 10-90% aqueous methanol over 4 minutes containing 0.1% TFA, 4 mL/min, monitoring at 220 nm), MS(ES): m/z=325.2 [M+H+]; 1H NMR (400 MHz, chloroform-d) δ 7.32 (dd, J=7.7, 1.5 Hz, 1H), 7.11 (dd, J=7.5, 1.5 Hz, 1H), 6.68-6.62 (m, 1H), 5.21 (br. s., 2H), 4.71 (s, 2H), 3.61 (s, 3H), 3.36 (s, 3H), 0.92 (s, 9H), 0.09 (s, 6H).

Provenance & Evidence