反应详情

A mixture of compound 1d (5.0 g, 21 mmol) and NaH (2.5 g, 64 mmol) in anhydrous THF (300 mL) was stirred at rt for 10 min. 2-Chloroquinoline (4.2 g, 25 mmol) was then added and the mixture was heated to 70° C. for 5 h. The reaction was quenched with brine (300 mL) and extracted with EtOAc (2×500 mL). The organic layer was washed with brine (300 mL), dried over Na2SO4 and concentrated under reduced pressure. The residue obtained was recrystallized with hot EtOAc-hexanes to give compound 31a. Mass Spectrum (LCMS, ESI pos.): Calcd. for C20H19N5O2: 362.1 (M+H). found: 362.2.

1. temperaturethe mixture was heated to 70° C. for 5 h
2. customThe reaction was quenched with brine (300 mL)
3. extractionextracted with EtOAc (2×500 mL)
4. washThe organic layer was washed with brine (300 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure
7. customThe residue obtained
8. customwas recrystallized with hot EtOAc-hexanes