反应详情

温度

80 °C

A mixture of (6Z)-5H-dipyrido[2,3-b:4′,3′-f]azepine-5,6(11H)-dione 6-oxime (1.00 g, 4.16 mmol), ammonium acetate (6.00 g, 77.8 mmol) and 3-(difluoromethyl)-5-methyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carbaldehyde (2.50 g, 8.19 mmol) in acetic acid (6.0 mL, 0.106 mol) was stirred at 80° C. for 2 h. The reaction was partitioned between dichloromethane/isopropanol (5:1) and water and the organic extract was washed with NaHCO3, brine, dried (MgSO4) and concentrated in vacuo. The residue was used in the next reaction without purification. Mass spec: (EI) m/z=466 (M+1).

1. customThe reaction was partitioned between dichloromethane/isopropanol (5:1) and water
2. extractionthe organic extract
3. washwas washed with NaHCO3, brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe residue was used in the next reaction without purification