反应详情

A solution of 2-trifluoromethyl-phenylhydrazine (1.1 g, 6.3 mmol) and 4,4,4-trifluoro-3-oxobutyronitrile (0.82 g, 6.0 mmol) in toluene (3 mL, anhyd.) was heated at reflux. After 5 h the reaction mixture was allowed to cool, concentrated and purified by chromatography (silica, EtOAc/Hex, 0:100 to 25:75) to yield the title compound (1.1 g, 61%) as an amber liquid. 1H-NMR (CD2Cl2): δ 8.40 (1H, br s), 7.77 (1H, d), 7.59 (2H, m), 7.17 (1H, m), 3.56 (2H, s); Rf 0.45 (20% EtOAc/Hex).

1. temperatureat reflux
2. temperatureto cool
3. concentrationconcentrated
4. custompurified by chromatography (silica, EtOAc/Hex, 0:100 to 25:75)