2-Iodophenol → HCID 11685541, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of compound 133 (1.75 g, 4.57 mmol), potassium carbonate (3.15 g, 22.85 mmol) in dimethylformamide (8 mL) was added 2-iodophenol (1.20 g, 5.48 mmol). It is heated to 80° C. for 12 hours with stirring under nitrogen atmosphere. The mixture was then cooled, diluted with water (20 mL) and extracted with EtOAc (2×20 mL). The combined organic layers were washed with water (2×10 mL), dried over anhydrous sodium sulphate and concentrated under vacuum. The residue thus obtained was purified by column chromatography (10-20% EtOAc-Hexane) to afford the title compound as white solid (2.45 g, 95%). mp 206-208° C.; HPLC: Inertsil ODS 3V (250×4.6 mm) 5 microns [solvent A=0.01 M KH2PO4 (pH 7.0); solvent B=CH3CN], Gradient elution program: T/% B=0/60, 5/60, 15/80, 30/80, 35/60, 40/60; 230 nm, Rt 26.65 min, 98.30% purity; MS (CI): m/z 566 (M+H, 100).

Provenance & Evidence