反应详情

To 2-amino-4-chloro-6-cyano-[1,3,5]triazine (Intermediate 3, 243 mg, 1.6 mmol) was added anhydrous DMF (5 mL), diisopropylethylamine (0.54 mL, 3.1 mmol) and N-methyl-aniline (184 mg, 1.7 mmol). The mixture was heated at 90 C in a pressure tube for 18 h before allowing to cool to room temperature. The reaction mixture was diluted with EtOAc (20 mL), washed with water (2×10 mL) and the organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to furnish the desired product which was used directly without further purification (138 mg, 39%). Method C HPLC-MS: MH+ requires m/z=227. Found: m/z=227, Rt=1.20 min (93%).

1. temperatureThe mixture was heated at 90 C in a pressure tube for 18 h
2. washwashed with water (2×10 mL)
3. dry with materialthe organic layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure