反应详情

A mixture of 1-(4-fluorophenyl)-5-isopropylpyrazol-4-amine (1.0 g, 4.54 mmol), 3-bromotetrahydrofuran-2-one (0.462 mL, 5.0 mmol) and AlMe3 (3.4 mL, 6.8 mmol, 2 M in toluene) in DCE (50 mL) was stirred for 2 hrs at rt followed by 45 min at 50° C. The mixture was then cooled to room temperature, quenched with 1N HCl (50 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/CH2Cl2 gradient elution) to give 2-bromo-N-[1-(4-fluorophenyl)-5-isopropylpyrazol-4-yl]-4-hydroxy-butanamide (1.38 g, 79%).

1. waitfollowed by 45 min at 50° C
2. temperatureThe mixture was then cooled to room temperature
3. customquenched with 1N HCl (50 mL)
4. extractionextracted with EtOAc (100 mL)
5. customThe organic layer was separated
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated in vacuo
8. custompurified by flash chromatography (SiO2, 0˜100% EtOAc/CH2Cl2 gradient elution)