Phosphorus oxychloride → HCID 58936497, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of (3-cyano-5-fluoro-6-hydroxy-pyridin-2-yl)-acetic acid methyl ester (9.10 g, 43.3 mmol), as prepared in the previous step, and POCl3 (40 mL, 433 mmol) was stirred at 95° C. for 7 h. The homogeneous brown solution was then concentrated under reduced pressure, and the residue was put on an ice bath, diluted with ether (200 mL), and then shaken with ice water (100 mL). The aqueous layer was extracted with ether (1×100 mL), and the organic layers were combined, dried (Na2SO4), and concentrated under reduced pressure at 40° C. to afford the title compound as a clear dark amber oil (9.45 g, 96%). 1H-NMR (300 MHz, CDCl3) δ 7.75 (d, 1H), 4.06 (s, 2H), 3.77 (s, 3H).

Provenance & Evidence