反应详情

温度

0 °C

To a suspension of (R)-ethyl 5-(2-(5-fluoro-2-oxo-1,2-dihydropyridin-3-yl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidine-3-carboxylate (0.73 g, 1.97 mmol) in DMF (10 mL) at 0° C. was added LiH (20 mg, 2.36 mmol). After stirring for 30 minutes, a solution of MeI (0.56 g, 3.93 mmol) in DMF (2 mL) was added and the reaction was stirred at ambient temperature for 17 hours. The reaction mixture was cooled to 0° C. and quenched with ice-water (30 mL). The mixture was extracted with EtOAc (3×), washed with water and brine, dried with MgSO4, filtered and concentrated. The crude material was purified by silica column chromatography, eluting with 2.5% MeOH/DCM to yield the title product (0.64 g, 85%). MS (apci) m/z=386.0 (M+H).

1. stirringthe reaction was stirred at ambient temperature for 17 hours
2. customquenched with ice-water (30 mL)
3. extractionThe mixture was extracted with EtOAc (3×)
4. washwashed with water and brine
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude material was purified by silica column chromatography
9. washeluting with 2.5% MeOH/DCM