反应详情

温度

90 °C

A microwave vial was charged with (2-aminopyridin-3-yl)(6-chloro-3-(trifluoromethyl)pyridin-2-yl)methanone (2.12 g, 7.028 mmol), potassium carbonate (1.166 g, 8.434 mmol), (S)-tert-butyl 2-isobutylpiperazine-1-carboxylate (1.874 g, 7.731 mmol) and dimethylformamide (4 mL). The reaction mixture was heated under microwave irradiation at 90° C. for 50 minutes. The reaction mixture was cooled down to room temperature and partitioned between a saturated solution of sodium bicarbonate and ethyl acetate. The organic extract was washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue was taken up in dichloromethane (50 ml) and trifluoroacetic acid (8 ml) was added. The reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was concentrated to dryness and partitioned between dichloromethane and a saturated solution of sodium carbonate. The organic extract was dried over magnesium sulfate, filtered and concentrated in vacuo. The residue was purified on silica gel by flash column chromatography to afford the title compound as a pale yellow oil (2.203 g, 77% yield).

1. temperatureThe reaction mixture was cooled down to room temperature
2. custompartitioned between a saturated solution of sodium bicarbonate and ethyl acetate
3. extractionThe organic extract
4. washwas washed with brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. additiontrifluoroacetic acid (8 ml) was added
9. concentrationThe reaction mixture was concentrated to dryness
10. custompartitioned between dichloromethane
11. extractionThe organic extract
12. dry with materialwas dried over magnesium sulfate
13. filtrationfiltered
14. concentrationconcentrated in vacuo
15. customThe residue was purified on silica gel by flash column chromatography