反应详情

温度

100 °C

3-Bromo-6-(trifluoromethyl)pyrazolo[1,5-a]pyrimidine (165 mg, 0.620 mmol), 5-ethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)thiophene-2-carboxylic acid (199 mg, 0.620 mmol), Pd2(dba)3 (56.8 mg, 0.062 mmol), tricyclohexylphosphine (43.5 mg, 0.155 mmol), and 1.27 M potassium phosphate tribasic (aq) (1.65 mL, 2.10 mmol) were placed in a sealed tube and purged with N2 for 5 min. The reaction was heated to 100° C. for 2 h. The reaction was then cooled to room temperature, diluted with water, and extracted with ethyl acetate 3×. The organic layers were combined, washed with brine, dried with sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by column chromatography (10-60% DCM/EtOAc). The fractions were combined and concentrated to give the title compound (95.0 mg, 0.278 mmol). LRMS (APCI) calc'd for (C14H10F3N3O2S) [M+H]+, 342.0; found 341.9.

1. custompurged with N2 for 5 min
2. temperatureThe reaction was then cooled to room temperature
3. additiondiluted with water
4. extractionextracted with ethyl acetate 3×
5. washwashed with brine
6. dry with materialdried with sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe residue was purified by column chromatography (10-60% DCM/EtOAc)
10. concentrationconcentrated