反应详情

Triethylamine (1.05 mL) is added drop wise to a mixture of (4-cyano-2-fluoro-benzaldehyde chlorooxime (600 mg) and 2-methoxyacrylate (421 mg) in dichloromethane (7.5 mL). The reaction mixture is stirred over night at room temperature. Water is added and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed with brine, dried over MgSO4, and concentrated in vacuo. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 80:20→50:50) to afford the title compound. LC (method 4): tR=0.93 min; Mass spectrum (ESI+): m/z=279 [M+H]+.

1. extractionthe aqueous phase is extracted with ethyl acetate
2. washThe combined organic phases are washed with brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo
5. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 80:20→50:50)