反应详情

770 mg (13.7 mmol) of iron powder were added to 1.7 g (4.6 mmol) of 2-(4-chloro-2-fluoro-5-hydroxy-6-nitrophenyl)-3-chloro-5-trifluoromethylpyridine in 9 ml of glacial acetic acid and 18 ml of methanol. The reaction mixture was refluxed for 15 hours with stirring and then concentrated under reduced pressure. The residue was taken up in 100 ml of ethyl acetate. Undissolved components were then filtered off. The filtrate was washed with 20 ml of water, dried over magnesium sulfate and finally concentrated. Yield: 96%; oil.

1. temperatureThe reaction mixture was refluxed for 15 hours
2. concentrationconcentrated under reduced pressure
3. filtrationUndissolved components were then filtered off
4. washThe filtrate was washed with 20 ml of water
5. dry with materialdried over magnesium sulfate
6. concentrationfinally concentrated