反应详情

温度

117.5 °C

2-(3-Methoxyphenyl)-cyclohexanone oxime, as described above in Step B, (0.62 g, 2.8 mmol) and polyphosphoric acid (20 g) were combined and heated at 115-120° C. with stirring for 20 min. The dark mixture was poured into ice (100 g) with stirring, diluted with H2O (200 mL), then extracted with CHCl3 (5×100 mL), the organic layers combined, washed with brine, dried (MgSO4), filtered, and concentrated to dryness to give the title compound after SiO2 chromatography (CHCl3:MeOH, 100:1 to 20:1).

1. stirringwith stirring
2. extractionextracted with CHCl3 (5×100 mL)
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated to dryness