反应详情

To a solution of 1-(2-fluorophenyl)-5-[3-fluoro-5-((R)-2,2,2-trifluoro-1-methylethoxymethyl)phenyl]-1H-pyrazol-3-ylamine (about 0.125 mmol) prepared in the previous step in dimethylformamide (0.5 ml) were sequentially added (S)-5-oxopyrrolidine-3-carboxylic acid (18 mg) prepared in Preparation 14 and WSC.HCl (29 mg) at room temperature, and the mixture was stirred for 3 hours. To this reaction mixture was added water, and the mixture was extracted with ethyl acetate. This organic layer was concentrated under reduced pressure, and the resulting residue was purified by silica gel thin-layer chromatography (eluent: chloroform/methanol=10/1). To the resulting solid were added water and a small amount of methanol, and the mixture was stirred. A solid was collected from this suspension by filtration, and was dried under reduced pressure to give the titled compound (32 mg).

1. extractionthe mixture was extracted with ethyl acetate
2. concentrationThis organic layer was concentrated under reduced pressure
3. customthe resulting residue was purified by silica gel thin-layer chromatography (eluent: chloroform/methanol=10/1)
4. additionTo the resulting solid were added water
5. stirringa small amount of methanol, and the mixture was stirred
6. filtrationA solid was collected from this suspension by filtration
7. customwas dried under reduced pressure