반응 #1582

반응 방정식

ethyl acetate

N-(4-chloro-2-fluoro-5-nitrophenyl)-1-cyclohexene-1,2-dicarboximide

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title product

N-(5-Amino-4-chloro-2-fluorophenyl)-1-cyclohexene-1,2-dicarboximide

용매

acetic acid

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   여과filtered through diatomaceous earth
3. 3
   농축The filtrate is concentrated in vacuo
4. 4
   기타to obtain a dark solid
5. 5
   여과is filtered through diatomaceous earth
6. 6
   기타the phases are separated
7. 7
   세척The organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine
8. 8
   건조dried over anhydrous magnesium sulfate
9. 9
   농축concentrated in vacuo

실험 절차

Iron powder (7.30 g, 130.7 mmol) is added portionwise to a mixture of N-(4-chloro-2-fluoro-5-nitrophenyl)-1-cyclohexene-1,2-dicarboximide (10.6 g, 32.7 mmol) in acetic acid (100 mL) at 65° C. After the addition is complete, the reaction mixture is stirred for 10 minutes, and filtered through diatomaceous earth. The filtrate is concentrated in vacuo to obtain a dark solid. A mixture of the solid in an ethyl acetate/saturated sodium hydrogen carbonate solution is filtered through diatomaceous earth, and the phases are separated. 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.

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