反应详情

温度

130 °C

A mixture of 4-methoxy-3-nitro-6,7-dihydro-5H-cyclopenta[b]pyridine (1.535 g, 7.905 mmol) in AcOH (2.6 mL) was treated 48% aq. HBr (2.6 mL, 23 mmol). The flask containing the mixture was sealed and heated at 130° C. for 40 min., then allowed to cool. The resulting mixture was concentrated under reduced pressure, the residue was neutralized to pH=7-8 using 50% NaOH with cooling. After further concentrating, the residue was diluted with MeOH and THF, dried, filtered and concentrated to give the crude sub-title compound as light brown powder, which was used without further purification. LCMS calc. for C8H9N2O3 (M+H)+: m/z=181.1. Found: 181.2.

1. additionThe flask containing the mixture
2. customwas sealed
3. temperatureto cool
4. concentrationThe resulting mixture was concentrated under reduced pressure
5. temperaturewith cooling
6. concentrationAfter further concentrating
7. additionthe residue was diluted with MeOH and THF
8. customdried
9. filtrationfiltered
10. concentrationconcentrated