反応 #1582

反応方程式

ethyl acetate

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

→

title product

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

溶媒

acetic acid

反応条件

後処理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   ろ過filtered through diatomaceous earth
3. 3
   濃縮The filtrate is concentrated in vacuo
4. 4
   その他to obtain a dark solid
5. 5
   ろ過is filtered through diatomaceous earth
6. 6
   その他the phases are separated
7. 7
   洗浄The organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine
8. 8
   乾燥dried over anhydrous magnesium sulfate
9. 9
   濃縮concentrated in vacuo

実験手順

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.

出典