反应详情

A solution Of (3S)-1-(2-chloropyrimidin-4-yl)-3-isopropyl-2-oxopyrrolidine-3-carbonitrile (55 mg) obtained in Step A of Example 9, 2-(4-amino-1H-pyrazol-1-yl)acetamide (35 mg) and acetic acid (13 μL) in ethanol (2 mL) was stirred in a microwave reactor at 150° C. for 1 hr, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH, ethyl acetate/methanol). The obtained crude product was subjected to HPLC (C18, mobile phase: water/acetonitrile (containing 0.1% ammonium formate)), to the obtained fraction was added saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. To a solution of the residue (17 mg) in ethanol (3 mL) was added 1M hydrochloric acid (57 μL), and the solvent was evaporated under reduced pressure. The residue was recrystallized (diisopropyl ether/ethanol) to give the title compound (13 mg).

1. customthe solvent was evaporated under reduced pressure
2. customThe obtained residue was purified by silica gel column chromatography (NH, ethyl acetate/methanol)
3. customThe obtained crude product
4. extractionthe mixture was extracted with ethyl acetate
5. dry with materialThe extract was dried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. additionTo a solution of the residue (17 mg) in ethanol (3 mL) was added 1M hydrochloric acid (57 μL)
8. customthe solvent was evaporated under reduced pressure
9. customThe residue was recrystallized (diisopropyl ether/ethanol)