反应详情

温度

130 °C

To a solution of [(R)-4-(3-bromo-5-trifluoromethyl-benzenesulfonylamino)-4,5,6,7-tetrahydro-indazol-1-yl]-acetic acid ethyl ester (Example 1-1, 100 mg, 0.196 mmol) in N,N-dimethylformamide (2 mL) in a microwave vial (5 mL), tetrakis(triphenylphosphine)palladium(0) (22 mg, 0.19 mmol), potassium tert-butoxide (45 mg, 0.4 mmol) and isopropenyl boronic acid pinacol ester (55 μl, 0.294 mmol) were added. After being heated in a microwave oven (130° C., 15 min.), the mixture was poured into aq. ammonium chloride (10 mL) and extracted with dichloromethane (20 mL×3). The combined organic layers were washed with water (10 mL×3) and brine (20 mL), dried over sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography (gradient elution, 0-5% methanol in dichloromethane) to afford [(R)-4-(3-isopropenyl-5-trifluoromethyl-benzene-sulfonylamino)-4,5,6,7-tetrahydro-indazol-1-yl]-acetic acid ethyl ester (34 mg, 36.8%) as a white solid, MS calcd. for C21H24F3N3O4S 471, obsd. (ESI+) [(M+H)+] 472.

1. extractionextracted with dichloromethane (20 mL×3)
2. washThe combined organic layers were washed with water (10 mL×3) and brine (20 mL)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was purified by column chromatography (gradient elution, 0-5% methanol in dichloromethane)