反应详情

A solution of 1-phenyl-2-(4-methoxyphenyl)-ethanone (Aldrich) (22.6 g, 0.1 mol), ethyl carbazate (12.5 g, 0.12 mol) and a spatula tip of TsOH in toluene (200 ml) was heated to reflux, and water was azeotropically removed. The reaction was complete (by TLC) after 4 hours. The solvent was removed under reduced pressure, and the crude solid was chromatographed, SiO2 (400 g), eluting with Hex/EtOAc, 7/3, affording 9 (24.0 g, 76.9%).

1. temperatureto reflux
2. customwater was azeotropically removed
3. customafter 4 hours
4. customThe solvent was removed under reduced pressure
5. customthe crude solid was chromatographed
6. washSiO2 (400 g), eluting with Hex/EtOAc, 7/3