反应详情

温度

60 °C

Into a flask was placed a suspension of iron (1.50 g, 26.9 mmol) (<10 μm) in ethanol (22 mL) δ 0 M hydrogen chloride in water (0.374 mL, 2.24 mmol) was added and the suspension was stirred for 2 h at 60° C. A solution of 5.0 M ammonium chloride in water (3.86 mL, 19.3 mmol) was added followed by a solution of 1-[4-chloro-3′,5′-difluoro-6-(hydroxyamino)-5-methylbiphenyl-2-yl]ethanone (1.4 g, 4.5 mmol) in ethanol (5.2 mL). The resulting suspension was stirred at 60° C. for 1 hour. The mixture was cooled, filtered and evaporated in vacuo. The residue was dissolved in a mixture of ethyl acetate and saturated sodium bicarbonate solution and stirred for a few minutes. The layers were separated and the ethyl acetate layer was washed with brine, dried over MgSO4 and evaporated in vacuo to give the desired product (0.95 g, 72%). LCMS calculated for C15H13ClF2NO (M+H)+: m/z=296.1. found: 296.0.

1. customInto a flask was placed
2. additionwas added
3. stirringThe resulting suspension was stirred at 60° C. for 1 hour
4. temperatureThe mixture was cooled
5. filtrationfiltered
6. customevaporated in vacuo
7. dissolutionThe residue was dissolved in a mixture of ethyl acetate and saturated sodium bicarbonate solution
8. stirringstirred for a few minutes
9. customThe layers were separated
10. washthe ethyl acetate layer was washed with brine
11. dry with materialdried over MgSO4
12. customevaporated in vacuo