反应详情

A solution of 3-nitro-6,7-dihydro-5H-cyclopenta[b]pyridin-4-ol (1.424 g, 7.904 mmol) in phosphoryl chloride (11.0 mL, 118 mmol) was heated at 110° C. in a sealed flask under nitrogen for 2 h. The mixture was cooled to room temperature, and concentrated under reduced pressure. The residue was carefully quenched with ice, and neutralized with 50% aq. NaOH to pH 7. The resulting mixture was extracted three times with EtOAc, dried, filtered and concentrated under reduced pressure to give the sub-title compound as a brown solid (0.82 g, 52%). LCMS calc. for C8H8N2O2(M+H)+: m/z=199.3. Found: 199.2.

1. concentrationconcentrated under reduced pressure
2. customThe residue was carefully quenched with ice
3. extractionThe resulting mixture was extracted three times with EtOAc
4. customdried
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure