反应详情

2,4-Dichloro-5-fluoro-3 amino-benzamide (6.00 g, 26.9 mmol) in THF (175 mL) is added dropwise to LiAlH4 (1 M in THF, 28.0 mL) in THF (175 mL). The reaction mixture is stirred for 1 h at rt and 5 h at reflux. Excess LiAlH4 is destroyed under cooling as described by L. F. Fieser & M. Fieser Vol 1, p 584 Wiley 1967. After 30 min the mixture is filtered, the filtrate is concentrated, diluted with Et2O and the precipitate is collected.

1. temperatureat reflux
2. customExcess LiAlH4 is destroyed
3. temperatureunder cooling
4. filtrationAfter 30 min the mixture is filtered
5. concentrationthe filtrate is concentrated
6. additiondiluted with Et2O
7. customthe precipitate is collected