反应详情

温度

80 °C

A mixture of 4-fluoro-3-nitrobenzonitrile (5.0 g, 30.1 mmol) and Fe powder (5.05 g, 90.3 mmol) in AcOH (100 mL) was heated at 80° C. for 1 hour under N2. Then the solvent was removed under vacuum and water (200 mL) was added to the residue. The solution was adjusted to pH 6 by addition of Na2CO3 and extracted with DCM (2×200 mL). The organic layers were combined, dried over Na2SO4, filtered and concentrated to yield 3-amino-4-fluorobenzonitrile (48), which was used without further purification. MS m/z 137.0 (M+1)+.

1. customThen the solvent was removed under vacuum and water (200 mL)
2. additionwas added to the residue
3. additionThe solution was adjusted to pH 6 by addition of Na2CO3
4. extractionextracted with DCM (2×200 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated