Lithium iodide → HCID 66801516, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of methyl 2-chloro-6-fluoro-4-iodo-benzoate (4.48 g, 14.2 mmol) in pyridine (28 mL) was added LiI (4.0 g, 29.9 mmol). The reaction mixture was heated at 115° C. for 4 hours. The solvent was removed under vacuum. The resultant solid was dissolved in water, and extracted with EtOAc. The aqueous layer was acidified with 1 N HCl to pH=4, extracted with EtOAc (3×30 mL). The combined organic phases were washed with 10% citric acid (2×30 mL), brine, dried (Na2SO4), filtered and concentrated to give the title compound (4.77 g, quantitative yield) as a yellow solid. 1H NMR (400 MHz, methanol-d4) δ 7.73 (s, 1H), 7.62 (dd, J=8.4, 1.1 Hz, 1H). LCMS (ESI) m/z 300.8 [M+H+].

Provenance & Evidence