反应详情

A mixture of 5,7-dichloro-6-(2,4,6-trifluorophenyl)[1,2,4]triazolo[1,5-a]pyrimidine (3.0 g, 9.4 mmol), (1S)-2,2,2-trifluoro-1-methylethylamine hydrogen chloride (4.2 g, 28.2 mmol), and N,N-diisopropylethylamine (4.9 mL, 28.2 mmol) in 100 mL of N,N-dimethylformamide is stirred at room temperature under nitrogen atmosphere for 13 h. The reaction mixture is diluted with ethyl acetate. The organic layer is washed with 1 N hydrochloric acid (2×) and saturated sodium chloride (2×), dried over magnesium sulfate, and concentrated to a residue. The residue is chromatographed over silica gel, eluting with 20% ethyl acetate in hexanes. Concentration provides 5-chloro-6-(2,4,6-trifluorophenyl)-N-[(1S)-2,2,2-trifluoro-1-methylethyl][1,2,4]triazolo[1,5-a]pyrimidin-7-amine as a light yellow solid (3.56 g). MS: m/z 396.0 (M+H).

1. washThe organic layer is washed with 1 N hydrochloric acid (2×) and saturated sodium chloride (2×)
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated to a residue
4. customThe residue is chromatographed over silica gel
5. washeluting with 20% ethyl acetate in hexanes
6. concentrationConcentration