反应详情

温度

65 °C

A mixture of N-(4-chloro-2-fluoro-5-nitrophenyl)-1-cyclohexene-1,2-dicarboximide (10.6 g, 32.7 mmol) in acetic acid is heated to 65° C., treated portionwise with iron powder (7.30 g, 130.7 mmol) over 40 minutes, stirred for 10 minutes, and filtered through diatomaceous earth. The resultant filtrate is washed with ethyl acetate, concentrated in vacuo, diluted with ethyl acetate and saturated sodium hydrogen carbonate solution, and filtered through a filter pad. The phases are separated and the organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product as a yellow solid (8.94 g, 94% yield, mp 164-165° C.).

1. filtrationfiltered through diatomaceous earth
2. washThe resultant filtrate is washed with ethyl acetate
3. concentrationconcentrated in vacuo
4. additiondiluted with ethyl acetate and saturated sodium hydrogen carbonate solution
5. filtrationfiltered through a filter pad
6. customThe phases are separated
7. washthe organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationconcentrated in vacuo