反应详情

4′-chloro-4-ethyl-2′-fluoro-3-nitrobiphenyl (1.795 g, 6.45 mmol) is suspended in a mixture of methanol (20 ml) and water (4 ml). To this mixture is added zinc dust (2.95 g, 45 mmol) and a solution of ammonium chloride (1.04 g, 19 mmol) in water (4 ml), and once the addition is complete the mixture is heated at reflux for 3 hours. The mixture is cooled to room temperature, and filtered through a plug of diatomaceous earth. The filtrate is partitioned between ethyl acetate and water, and the organic extract is washed with brine, dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated under reduced pressure to give 4′-chloro-4-ethyl-2′-fluorobiphen-3-ylamine (1.546 g), used without further purification in the next step.

1. temperatureis heated
2. temperatureat reflux for 3 hours
3. filtrationfiltered through a plug of diatomaceous earth
4. customThe filtrate is partitioned between ethyl acetate and water
5. extractionthe organic extract
6. washis washed with brine
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. customthe filtrate is evaporated under reduced pressure