反应详情

Dissolve bromomalonaldehyde (Aldrich; 2.5 g, 16.5 mmol) and 3-aminopyrazole (Aldrich; 1.38 g, 16.5 mmol) in glacial acetic acid (25 mL) and reflux the resulting mixture under nitrogen for 2 h. Concentrate under reduced pressure. Dissolve the residue in absolute methanol (150 mL), vacuum filter through a pad diatomaceous earth and concentrate under reduced pressure. Chromatograph on flash silica using a gradient from neat hexane to 50% ethyl acetate/50% hexane to obtain 365 mgs (11%) of the subtitled compound as a light yellow solid. High Resolution Mass Spectrum: 197.9674 (M+1).

1. temperaturereflux the resulting mixture under nitrogen for 2 h
2. concentrationConcentrate under reduced pressure
3. dissolutionDissolve the residue in absolute methanol (150 mL)
4. filtrationvacuum filter through a pad diatomaceous earth
5. concentrationconcentrate under reduced pressure