HCID 69968949, compound → HCID 22997650, compound

Participants

Reaction Steps

(5-Iodothiophen-2-yl)-oxo-acetic acid ethyl ester (0.298 g, 0.96 mmol) was dissolved in 1,4 dioxane (4 ml) and 20% KOH (0.5 ml). The reaction mixture was stirred at ambient temperature for 4 hours then volatile solvent was removed by rotary evaporation. The residue was dissolved in 5 ml water and extracted with diethyl ether (35 ml). The aqueous layer was acidified to pH 3-4 with glacial acetic acid, and extracted with ethyl acetate (3×35 ml). The combined ethyl acetate extracts were dried over Na2SO4 and concentrated under vacuum to provide Preparation 1c (92 mg, 34%). MS (M−H)−: 280.77; 1H NMR (300 MHz, DMSO-d6) δ7.59 (1H, d, J=3.9 Hz), 7.50 (1H, d, J=4.0 Hz).

Provenance & Evidence