تفاعل #1582

معادلة التفاعل

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

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONAfter the addition
2. 2
   ترشيحfiltered through diatomaceous earth
3. 3
   تركيزThe filtrate is concentrated in vacuo
4. 4
   أخرىto obtain a dark solid
5. 5
   ترشيحis filtered through diatomaceous earth
6. 6
   أخرىthe phases are separated
7. 7
   غسيلThe organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine
8. 8
   تجفيفdried over anhydrous magnesium sulfate
9. 9
   تركيزconcentrated in vacuo

الإجراء التجريبي

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.

المصدر