反应详情

A mixture of N-[(1S,2S)-2-{[3-bromo-5-(trifluoromethyl)pyridin-2-yl]amino}cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide (Example 107; 67 mg, 0.14 mmol), methylboronic acid (CAS number 13061-96-6; 24 mg, 0.41 mmol), tetrakis(triphenylphosphine)palladium (16 mg, 0.014 mmol) and potassium carbonate (aq. 2 M, 271 μl, 0.54 mmol) in 1,4-dioxane (450 μl) was sealed, evacuated and purged with nitrogen and then subjected to microwave irradiation at 140° C. for 30 minutes. The reaction was partitioned between ethyl acetate and water, washing with water, brine, dried over magnesium sulfate and concentrated in vacuo. This was then purified by reverse phase preparative HPLC (eluted with acetonitrile/water containing 0.1% ammonia) to afford the title compound.

1. customwas sealed
2. customevacuated
3. custompurged with nitrogen
4. customirradiation at 140° C. for 30 minutes
5. customThe reaction was partitioned between ethyl acetate and water
6. washwashing with water, brine
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated in vacuo
9. customThis was then purified by reverse phase preparative HPLC (eluted with acetonitrile/water containing 0.1% ammonia)