反应详情

A solution of 4-[(2-oxocyclohexyl)methyl]-benzonitrile (7 g) (0.033 mol) and anhydrous N,N-dimethylhydrazine (9.2 ml) (3,7 eq.) in EtOH (100 ml) was refluxed for 8 h. After cooling, the reaction mixture was concentrated to dryness. The residue was partitioned between tBuOMe and water, the organic phase washed twice with water, dried over magnesium sulfate, and concentrated to yield 4-[[2-(dimethylhydrazono)cyclohexyl]methyl]-benzonitrile (6.1 g) as a orange oil. 1H NMR (CDCl3): 7.55 (2H, d), 7.30 (2H, d), 3.15 (1H, dd), 2.9-2.15 (6H, m), 2.3 (6H, s), 1.8-1.3 (4H, m).

1. temperatureAfter cooling
2. concentrationthe reaction mixture was concentrated to dryness
3. customThe residue was partitioned between tBuOMe and water
4. washthe organic phase washed twice with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated