反应详情

温度

150 °C

[2-(3-Chloro-2-fluoro-phenyl)-ethylamine]-carbamic methyl ester (890 mg, 3.85 mmol) and polyphosphoric acid (15 mL) were added to a 1-L, round bottom flask equipped with a magnetic stirring bar and reflux condenser. The reaction mixture was heated in an oil bath at 140-160° C. for 2 hours while keeping vigorous stirring. The reaction mixture was then allowed to cool to room temperature and poured into H2O (100 mL). After extraction with EtOAc, the organic layer was washed with brine, dried over anhy. MgSO4, filtered and concentrated to give a yellowish oil which was crystallized from Et2O to give title compound as a white solid (30 mg, 4%). MS: 200.1 (M+H)+.

1. customequipped with a magnetic stirring bar
2. temperaturereflux condenser
3. temperatureto cool to room temperature
4. extractionAfter extraction with EtOAc
5. washthe organic layer was washed with brine
6. customdried over anhy
7. filtrationMgSO4, filtered
8. concentrationconcentrated
9. customto give a yellowish oil which
10. customwas crystallized from Et2O