反应详情

温度

100 °C

To a stirred solution of 72 (681 mg, 2.72 mmol) in DMF (9.894 mL) was added potassium carbonate (855 mg, 6.18 mmol), and then 5-(furan-2-yl)-3-(trifluoromethyl)-1H-pyrazole (500 mg, 2.474 mmol) [made by following the procedure described above for the synthesis of compound 14 (scheme 2, example 1c, step 4), except using hydrazine hydrate instead of 13 as the starting material]. The resulting solution was allowed to stir at 100° C. for 1 h. The mixture was quenched with water and extracted with ethyl acetate, washed with brine, dried (MgSO4) filtered and concentrated. The residue was purified by silica gel column chromatography with gradient of EtOAc (10-20%) in hexanes to afford 73 (340 mg, 37%) as a colorless oil. LRMS (ESI): calc. 371.1; found 394.0 (MNa)+.

1. customThe mixture was quenched with water
2. extractionextracted with ethyl acetate
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography with gradient of EtOAc (10-20%) in hexanes