反应详情

温度

125 °C

6-Methoxyanthranilonitrile (14.0 g) was dissolved in nitrobenzene (150 ml) and cyclohexanone (18.45 g), and freshly fused zinc chloride (25.6 g) was added. The reaction mixture was warmed at 125° C. for 1.5 hr, cooled to room temperature, and poured into ether (1 l). The solid was collected, washed with ether, and distributed between 2-butanone and ammonium hydroxide. The organic phase was washed with brine, dried, filtered, and evaporated. The residue was recrystallized two times from ethyl acetate to give 13.7 g (63.8%), mp 187°-188° C.

1. temperaturecooled to room temperature
2. customThe solid was collected
3. washwashed with ether
4. washThe organic phase was washed with brine
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe residue was recrystallized two times from ethyl acetate
9. customto give 13.7 g (63.8%), mp 187°-188° C.