反应详情

To a suspension of 2,5-dimethyl-4H-pyrazolo[1,5-a]pyrimidin-7-one (10.0 g, 61.3 mmol) in toluene (150 mL), add N,N-dimethylaniline (9.7 mL, 76.7 mmol). Add phosphorus oxychloride (11.2 mL, 122.6 mmol) dropwise to this white suspension. Reflux for 3 h under an inert atmosphere, cool to room temperature, and concentrate the reaction to a brown oil using reduced pressure. Dissolve the oil in ethyl acetate (250 mL) and basify with 1 N NaOH. Separate and extract the basic aqueous phase with additional ethyl acetate (2×100 mL). Combine the organic phases, dry over anhydrous magnesium sulfate, filter, and concentrate under reduced pressure to yield a brown solid. Purify the material using flash chromatography, eluting with 80% hexane/20% (30% THF/hexane) to 0% hexane/100% (30% THF/hexane) in a step gradient of 20% increments to provide a light green solid (6.65 g, 59%). ES/MS m/z (35Cl) 182.3 (M+1)+.

1. temperatureReflux for 3 h under an inert atmosphere
2. concentrationconcentrate
3. customthe reaction to a brown oil
4. customSeparate
5. extractionextract the basic aqueous phase with additional ethyl acetate (2×100 mL)
6. dry with materialCombine the organic phases, dry over anhydrous magnesium sulfate
7. filtrationfilter
8. concentrationconcentrate under reduced pressure
9. customto yield a brown solid
10. customPurify the material
11. washeluting with 80% hexane/20% (30% THF/hexane) to 0% hexane/100% (30% THF/hexane) in a step gradient of 20% increments