反应详情

温度

60 °C

To a suspension of CDI (0.949 g, 5.86 mmol) in THF (10 mL) was added 3-trifluoromethyl-5,6,7,8-tetrahydro-[1,6]naphthyridine (0.988 g, 4.88 mmol) and the reaction mixture was heated at about 60° C. for about 16 h. The reaction mixture was cooled at ambient temperature and concentrated in vacuo to afford a light orange solid. The residue was dissolved in DCM (10 mL), washed with water (2×10 mL), and the organic portion was separated, dried over MgSO4, filtered, and concentrated in vacuo to give imidazol-1-yl-(3-trifluoromethyl-7,8-dihydro-5H-[1,6]naphthyridin-6-yl)-methanone (1.28 g, 88%) as a yellow solid which was used in subsequent reactions without further purification. RP-HPLC (Table 1, Method d) Rt 2.10 min; m/z: (M+H)+ 297.

1. temperatureThe reaction mixture was cooled at ambient temperature
2. concentrationconcentrated in vacuo
3. customto afford a light orange solid
4. washwashed with water (2×10 mL)
5. customthe organic portion was separated
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo