反应详情

To a mixture of 4-methyl-3-oxopentanenitrile (0.9 g, 0.008 mole) in ethyl alcohol (5 mL) was added hydrazine (0.25 mL, 0.008 mole). The reaction mixture was refluxed for 1 hour and then cooled to room temperature. The reaction mixture was concentrated and the residue was dissolved in MeOH (2 mL). The crude product was loaded on a sulfuric acid bound resin (AG 50W-X2, hydrogen form, 100-200 mesh, BioRad), washed with MeOH (50 mL), then washed with 2N NH3 in methanol (10 mL). The ammonia washes were combined and concentrated to afford the desired product (700 mg, 68%). 1HNMR (400 MHz, MeOD) δ 5.44 (s, 1H), 2.84-2.90 (m, 1H), 1.24 (d, J=6.4 Hz).

1. temperatureThe reaction mixture was refluxed for 1 hour
2. concentrationThe reaction mixture was concentrated
3. dissolutionthe residue was dissolved in MeOH (2 mL)
4. washwashed with MeOH (50 mL)
5. washwashed with 2N NH3 in methanol (10 mL)
6. concentrationconcentrated