反应详情

温度

120 °C

Into a Vial was added the 5-Bromo-pyridine-2-sulfonic acid thiazol-2-ylamide (50 mg, 0.0002 mol), 9,9-DIMETHYL-4,5-BIS(DIPHENYLPHOSPHINO)XANTHENE (11 mg, 0.000019 mol), Tris(dibenzylideneacetone)dipalladium(0) (5.7 mg, 0.0000062 mol), 1-(4-Chloro-benzyl)-1H-pyrazol-4-ylamine (39 mg, 0.00019 mol) and N,N-Dimethylacetamide (2.1 mL, 0.022 mol). The mixture was sparged with argon for ˜5 min. Sodium tert-butoxide (75 mg, 0.00078 mol) was added and the reaction mixture was heated at 120° C. for 30 min in microwave. The reaction mixture was filtered through celite. The filtrate was diluted with Ethyl acetate and washed with 0.1 N HCl solution, water (3×) and brine, dried over sodium sulfate, filtered and was concentrated to give the crude product that was purified on ISCO (40% to 100% Ethyl acetate). 16.8 mg of the product was obtained as a light tan solid.

1. customThe mixture was sparged with argon for ˜5 min
2. filtrationThe reaction mixture was filtered through celite
3. additionThe filtrate was diluted with Ethyl acetate
4. washwashed with 0.1 N HCl solution, water (3×) and brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationwas concentrated
8. customto give the crude product that
9. customwas purified on ISCO (40% to 100% Ethyl acetate)