反应详情

A mixture of tert-butyl N-[(1S,2S)-2-{[3-bromo-5-(trifluoromethyl)pyridin-2-yl]amino}cyclopentyl]carbamate (1.26 g, 2.96 mmol), methylboronic acid (CAS number 13061-96-6; 0.532 g, 8.88 mmol), tetrakis(triphenylphosphine)palladium (0.342 g, 0.296 mmol) and potassium carbonate (1.303 g, 9.43 mmol) in 1,4-dioxane (10 ml) and water (1.5 ml) was sealed, evacuated and purged with nitrogen and subjected to microwave irradiation at 140° C. for 1 hour. The mixture was partitioned between ethyl acetate (10 ml) and water (10 ml). The organics were extracted with ethyl acetate (2×20 ml). The combined organics were washed with brine (20 ml), filtered through a hydrophobic frit and concentrated in vacuo. The crude product was purified by column chromatography (silica, 0-60% ethyl acetate/petrol) to afford the title compound.

1. customwas sealed
2. customevacuated
3. custompurged with nitrogen
4. customirradiation at 140° C. for 1 hour
5. customThe mixture was partitioned between ethyl acetate (10 ml) and water (10 ml)
6. extractionThe organics were extracted with ethyl acetate (2×20 ml)
7. washThe combined organics were washed with brine (20 ml)
8. filtrationfiltered through a hydrophobic frit
9. concentrationconcentrated in vacuo
10. customThe crude product was purified by column chromatography (silica, 0-60% ethyl acetate/petrol)