反应详情

温度

130 °C

(E)-1-(2-hydroxy-3-methylphenyl)ethanone O-acetyl oxime (Step 46.3) (6.0 g, 29.0 mmol) was dissolved in pyridine (60 mL) and the resulting mixture was heated up and stirred at 130° C. for 40 hr, cooled down to RT and concentrated under reduced pressure. The crude product was purified by silica gel column chromatography (hexane/EtOAc 0-50% EtOAc) to afford the title product (3.62 g, 23.12 mmol, 80% yield) as pale yellow oil. tR: 0.96 min (LC-MS 2); ESI-MS: 148 [M+H]+; Rf=0.56 (hexane/EtOAc 3:1).

1. temperaturethe resulting mixture was heated up
2. temperaturecooled down to RT
3. concentrationconcentrated under reduced pressure
4. customThe crude product was purified by silica gel column chromatography (hexane/EtOAc 0-50% EtOAc)