Sodium Hydroxide → HCID 16065089, compound

Participants

Reaction Steps

To a stirred solution of 81 (412 mg, 0.99 mmol) in EtOH (10 mL) was added 10% aqueous NaOH (5 mL) and the reaction mixture heated to reflux. After 2 h, the solution was cooled to r.t., and the mixture concentrated to 5 mL under reduced pressure. Acetic acid was then added dropwise with stirring until a precipitate appeared, which was filtered off and dried to afford 82 (267 mg, 0.89 mmol, 90%) as a yellow powder. 1H NMR (400 MHz, DMSO-d6) δ 0.91 (d, J=6.6 Hz, 2H), 1.92 (nonet, J=6.6 Hz, 1H), 2.60 (d, J=7.2 Hz, 2H), 7.69 (s, 1H), 7.95 (s, 1H), 8.08 (d, J=1.9 Hz, 1H), 8.27 (s, 1H), 11.73 (s, 1H).

Provenance & Evidence