4-Fluoro-5-iodo-2-methylphenol synthesis

Yield:900175-53-3 84%

Reaction Conditions:

with sodium hydroxide in methanol;water at 0; for 2 h;

Steps:

122.C

[00412] To 122B (4.2g, 7.9mmol) in methanol (20 mL) was added NaOH (0.63 g as a 50% aqueous solution) at 0⁰C. After TLC (10% EtOAc/Hexane) indicated the reaction was complete (2 h at 0⁰C)₅ the mixture was diluted with EtOAc, and washed with water and brine. The organic layer was dried over MgSθ4 and concentrated. The crude product was purified by silica gel chromatography to give 122C (3.36g, 84% yield) as a solid. ¹H NMR (400 MHz, CDCl₃) δ ppm 2.19 (s, 3 H) 4.87 (s, 1 H) 6.83 (d, J=8.35 Hz, 1 H) 7.10 (d, J=5.27 Hz, 1 H).

References:

WO2006/76246,2006,A2 Location in patent:Page/Page column 207