tert-Butanol → HCID 68779984, compound

Participants

Reaction Steps

A solution of monomethyl 2-fluoroisophthalate (0.4 g) in tert-butyl alcohol (10 mL) was treated with Et3N (0.56 mL) and diphenylphosphoryl azide (0.75 mL). After 1 h, the mixture was heated at reflux for 24 h, then cooled and concentrated. The residue was diluted with EtOAc, washed with saturated aqueous NaHCO3, dried over MgSO4, filtered, and evaporated. Silica gel chromatography (acetone/hexane gradient) provided the product. 1H-NMR (CDCl3): δ 8.31 (1H, br t, J=7.2 Hz), 7.55 (1H, ddd, J=1.6, 6.8, 8.0 Hz), 7.16 (1H, ddd, J=1.2, 8.0, 8.0 Hz), 6.80 (1H, br s), 3.93 (3H, s), 1.54 (9H, s).

Provenance & Evidence