反应详情

温度

60 °C

To a solution of 2,5,6-trichloronicotinonitrile (Method 44, 1.0 g, 4.8 mmol) and DIEA (0.81 g, 6.2 mmol) in n-BuOH (5 ml) was added 5-cyclopropyl-1H-pyrazol-3-amine (2.3 g, 19.3 mmol). The reaction was heated to 60° C. for 2 hours, at which point the reaction was cooled to room temperature and concentrated. The resulting residue was diluted with 10 ml ACN, and stored at 0° C. for 1 hour. The solids that formed were then filtered, washed with cold ACN, dried and collected to give the title compound (0.62 g, 43%). MS: Calcd.: 294. Found: [M+H]+ 295.

1. temperaturewas cooled to room temperature
2. concentrationconcentrated
3. additionThe resulting residue was diluted with 10 ml ACN
4. customThe solids that formed
5. filtrationwere then filtered
6. washwashed with cold ACN
7. customdried
8. customcollected