反应详情

温度

60 °C

A mixture of 3-bromo-1-[1-(4-fluorophenyl)-5-isopropylpyrazol-4-yl]pyrrolidin-2-one (0.023 g, 0.063 mmol), 5-methyl-3-(trifluoromethyl)-1H-pyrazole (0.040 g, 0.27 mmol) and K2CO3 (0.060 g, 0.43 mmol) in DMF (1 mL) was stirred at 60° C. for 1 hr. It was then cooled to room temperature, quenched with water (30 mL) and extracted with EtOAc (100 mL). The organic layer was separated, dried over anhydrous sodium sulfate, concentrated in vacuo and purified by flash chromatography (SiO2, 0˜100% EtOAc/hexanes gradient elution) to give the title compound (0.022 g, 80%). 1H NMR (400 MHz, CDCl3) δ 7.52 (s, 1H), 7.37 (dd, J=9.2, 4.8 Hz, 2H), 7.17 (dd, J=8.6, 8.6 Hz, 2H), 6.32 (s, 1H), 5.05 (dd, J=9.2, 5.6 Hz, 1H), 4.07 (m, 1H), 3.80 (m, 1H), 2.84-3.02 (m, 2H), 2.74 (m, 1H), 2.45 (s, 3H), 1.21 (d, J=7.6 Hz, 3H), 1.11 (d, J=6.8 Hz, 3H); MS: (ES) m/z calculated for C21H21F4N5O [M+H]+ 436.1. found 436.1.

1. temperatureIt was then cooled to room temperature
2. customquenched with water (30 mL)
3. extractionextracted with EtOAc (100 mL)
4. customThe organic layer was separated
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated in vacuo
7. custompurified by flash chromatography (SiO2, 0˜100% EtOAc/hexanes gradient elution)