反应详情

A suspension of pyridinium chlorochromate (47.5 g, 0.22 mol) and neutral alumina (170 g) in dichloromethane (600 ml) is stirred for 30 minutes at room temperature. 2-[(2,3-dimethylphenyl) amino]benzyl alcohol (25 g, 0.11 mol) is added and the reaction mixture is stirred at room temperature overnight. The suspension is filtered through a pad of silica gel (1000 g) and the product is eluted with dichloromethane (2500 ml). The combined filtrate and eluant are evaporated and the residue is recrystallized from cold methanol/water to give 2-[(2,3-dimethylphenyl)amino]benzaldehyde (11.95 g, Recrystallization from hexane at 0° C. gives analytical material; mp 45°-47° C.

1. stirringthe reaction mixture is stirred at room temperature overnight
2. filtrationThe suspension is filtered through a pad of silica gel (1000 g)
3. washthe product is eluted with dichloromethane (2500 ml)
4. customThe combined filtrate and eluant are evaporated
5. customthe residue is recrystallized from cold methanol/water