反应详情

温度

70 °C

Intermediate 5.64 (41 mg, 0.093 mmol) was dissolved in TFA (1.5 mL) and the resulting solution was heated to 70° C. After stirring 6.5 h, the reaction mixture was cooled and concentrated in vacuo. The resulting residue was partitioned between EtOAc, water, and brine. The phases were separated, and the aqueous phase was extracted with EtOAc. The combined organic phase was dried over Na2SO4, filtered, and concentrated to afford crude 6-chloro-4-((R)-1-((R)-5-oxopyrrolidin-3-yl)ethoxy)pyrazolo[1,5-a]pyrazine-3-carbonitrile (5.65) that was used without further purification. LCMS-ESI+ (m/z): [M+H]+ calcd for C13H13ClN5O2: 306.1; found: 305.8.

1. temperaturethe reaction mixture was cooled
2. concentrationconcentrated in vacuo
3. customThe resulting residue was partitioned between EtOAc, water, and brine
4. customThe phases were separated
5. extractionthe aqueous phase was extracted with EtOAc
6. dry with materialThe combined organic phase was dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated